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                《化學試劑》2022年第9期中英文摘要(附整期文章PDF文檔)

                CeO2納米酶活性與抗菌性能研究進展

                 

                郭佳靖,高艷芳,張欣*

                (內蒙古工業大學 化工學院,內蒙古 呼和浩特  010051

                 

                摘要:近年來,細菌多重耐藥性(Multidrug Resistance,MDR)現象日益嚴重,已威脅到人類健康。納米材料的出現,為這一難題的解決帶來希望。其中,二氧化鈰納米顆粒(Cerium Oxide Nanoparticles,CeO2 NPs)作為一種新型抗菌劑,具有生產成本低、結構穩定性高、催化活性可調、生物安全性高等優點,因而具有重要研究價值。根據Ce3+Ce4+含量比值變化,CeO2 NPs可表現出不同納米酶活性,進而可調節生物體內活性氧(Reactive Oxygen Species,ROS)自由基的水平,從而有效殺死細菌,破壞其細胞結構。綜述CeO2 NPs用于多種模式微生物的抗菌性能,闡述其抗菌機理,分析不同因素對其抗菌性能的影響,并對其在抗菌領域的應用前景進行展望,期望對抗菌劑的開發和應用提供更多參考。

                關鍵詞:二氧化鈰納米顆粒;抗菌機理;納米酶活性;活性氧物種;耐藥性

                中圖分類號:O69     文獻標識碼:A       文章編號:0258-32832022

                 

                The Application Progress of Cerium Oxide Nanozyme Activities and Antibacterial Properties GUO Jia-jing, GAO Yan-fang, ZHANG Xin* (College of Chemical Engineering, Inner Mongolia University of Technology, Inner Mongolia Hohhot, 010051, China), Huaxue Shiji, 2022,449

                Abstract: In recent years, bacterial multidrug resistance (MDR) has become increasingly serious, which has threatened human health. The emergence of nanomaterials brings hope for the solution of this difficult problem. Cerium oxide nanoparticles (CeO2 NPs) as a new antibacterial agent, has the advantages of low production cost, high structural stability and adjustable catalytic activity and thus shows substantial research value. CeO2 NPs show different enzyme activities according to the content of Ce3+ and Ce4+, which then could regulate the level of reactive oxygen species (ROS) free radicals, so as to effectively kill bacteria and destroy their cell structure. In this review, we mainly summarize the reports on antibacterial performance of CeO2 NPs against various model bacteria, and its antibacterial mechanism is elaborated in detail. The effects of diversely influence factors on antibacterial properties were also discussed. Finally, the application prospect of this antibacterial material was put forward, wishing to provide more reference for the development and application of antibacterial agents.

                Key words: cerium oxide nanoparticles; antibacterial mechanism; enzyme-like activity; reactive oxygen species; drug resistanc

                引用本文:郭佳靖, 高艷芳, 張欣. CeO2納米酶活性與抗菌性能研究進展[J]. 化學試劑, 2022,449:1249-1256.

                 

                植物酯酶應用于農藥殘留檢測的研究進展

                羅俊霞1,趙建波*2,張潔*2,張剛3,劉青4,潘玲1,馬蕾2,王倩2,張威3

                1.鄭州市農產品質量檢測流通中心,河南 鄭州  450006;2.鄭州市農業技術推廣中心,河南 鄭州  450002;3.河南恒晟檢測技術有限公司,河南 新鄭  451100;4.鄭州市農業綜合行政執法支隊,河南 鄭州  450002

                 

                摘要為了全面了解植物酯酶在農藥殘留快速檢測中的應用,通過閱讀大量國內外相關文獻,從植物酯酶及其制備、純化、固定方法,植物酯酶對各種條件的篩選及其應用于農藥殘留檢測時檢測結果的準確性及預防措施等幾方面進行了歸納,總結了植物酯酶應用于農藥殘留檢測新方法,指出了植物酯酶應用于農藥殘留檢測存在的問題。盡管如此,由于酶抑制法可對農藥殘留進行高通量快速篩查,植物酯酶又具有較高的性價比,因此,該酶具有無可取代的地位和作用。呼吁盡快制定植物酯酶抑制法農藥殘留快速檢測試劑的制備標準,促使植物酯酶更好地應用于農藥殘留快速檢測工作中。

                關鍵詞植物酯酶;酶活;酶抑制法;快速檢測;農藥殘留

                中圖分類號O656.31            文獻標識碼A   文章編號:0258-32832022 

                 

                Research Progress of Plant Esterase in the Detection of Pesticide Residues LUO Jun-xia1, ZHAO Jian-bo*2, ZHANG Jie*2, ZHANG Gang3, LIU Qing4, PAN Ling1, MA Lei2, WANG Qian2 ,ZAHNG Wei3(1. Zhengzhou Agricultural Product Quality Testing and Distribution Center, Zhengzhou 450006, China; 2. Zhengzhou Agricultural Technology Extension Centre, Zhengzhou 450006, China; 3.Henan Hengsheng Testing Technology Co., Ltd., Xinzheng 451100, China; 4. Zhengzhou Agricultural Comprehensive Administrative Law Enforcement Detachment, Zhengzhou 450002, China), Huaxue Shiji,

                Abstract: In order to fully understand the application of plant esterase in the rapid detection of pesticide residues, we summarized the methods for preparation, purification and fixation of plant esterase, and the screening of various conditions and the accuracy of sensing results and preventive strategies of plant esterase when applied for the detection of pesticide residues on the basis of a large number of related literature at home and abroad in this review. Moreover, the new methods of applying plant esterase for the detection of pesticide residues were summed up, and their existing problems in the application of plant esterase to the detection of pesticide residues were discussed as well. Nevertheless, the plant esterase has an irreplaceable position and role due to its cost-effective performance as well as high-throughput screening of pesticide residues by enzymatic inhibition method. In the purpose of promoting the application of plant esterase in the rapid detection of pesticide residues, it is significant to set industrial chain standard for rapid detection of pesticide residues by plant esterase inhibition.

                Key words: plant esterase; the activity of enzyme; enzyme inhibition method; rapid detection; pesticide residue

                引用本文:羅俊霞,李潤培,趙建波,等.植物酯酶應用于農藥殘留檢測的研究進展[J].化學試劑,2022,449:1257-1265.

                 

                NO供體型丹皮酚氧異丁酸硝酸酯類衍生物的合成及降血脂活性研究

                李光耀1,陳誠1,卞在東1,劉鵬1,徐淼焱1,黃鵬*1,2

                1.安徽中醫藥大學 藥學院,安徽 合肥  230012;2.中藥研究與開發安徽省重點實驗室,安徽 合肥  230012

                 

                摘要:以丹皮酚為先導化合物,與α-溴代異丁酸通過Willamson合成法得到丹皮酚氧異丁酸,與不同碳數的二溴烷烴生成丹皮酚氧異丁酸溴代烷基酯中間體,再與硝酸銀反應得到5個目標化合物。目標化合物結構經核磁共振氫譜、紅外光譜和質譜確證。采用HepG2高血脂細胞實驗、脂肪酶活性抑制和膽酸鹽結合能力實驗對所得化合物進行活性研究。實驗結果表明目標化合物降血脂活性高于丹皮酚,其中丹皮酚氧異丁酸硝氧乙基酯活性最好,其升高HDL-C能力高于非諾貝特。當目標化合物濃度為5 mg/mL時,脂肪酶抑制率可達40%左右,對甘氨膽酸鈉(SG)、牛黃膽酸鈉(ST)的結合率可達80%左右。

                關鍵詞:丹皮酚;苯氧芳酸;合成;降血脂活性

                中圖分類號:TQ460.1    文獻標識碼:A      文章編號:0258-3283(2022)

                 

                Synthesis and Hypolipidemic Activity of NO-donating Paeonoloxyisobutyrate Nitrate Derivatives LI Guang-yao1, CHEN Cheng1, BIAN Zai-dong1, LIU Peng1,XU Miao-yan1, HUANG Peng*1,2 (1.School of Pharmacy, Anhui University of Chinese Medicine, Hefei 230012, China; 2.Anhui Province Key Laboratory of Research & Development of Chinese Medicine, Hefei 230012, China) , Huaxue Shiji,2022,44 (9),00 ~ 00

                AbstractPaeonol oxyisobutyric acid was synthesized from paeonol and α-bromoisobutyric acid by Willamson method, and then reacted with dibromoalkanes with different carbon numbers to form paeonol oxyisobutyric acid alkyl ester intermediate. The intermediate is then reacted with silver nitrate to obtain five target compounds  The structure of the target compound was confirmed by 1HMNR, IR and MS. The target compounds were subjected to activity studies by using HepG2 hyperlipidemia assay, lipase activity inhibition and cholate binding capacity assay. The HepG2 experimental results showed that the lipid-lowering activities of target compounds were higher than that of paeonol, among which 3a had the best activity. Moreover, the ability to increase HDL-C of target compound was higher than that of fenofibrate, and the inhibition rate of lipase was about 40%, the binding rate to sodium glycocholate (SG) and sodium taurocholate (ST) can reach about 80%, when the concentration of target compound was 5 mg/mL.

                Key wordspaeonol; phenoxyaromatic acid; synthesis; hypolipidemic activity

                引用本文:李光耀,陳誠,卞在東,等. NO供體型丹皮酚氧異丁酸硝酸酯類衍生物的合成及降血脂活性研究 [J]. 化學試劑, 2022, 44(9): 1266-1271。

                 

                 

                基于Click反應的5-氟尿嘧啶與4-苯胺喹唑啉骨架的拼接合成及其抗腫瘤活性評價

                 

                梁光平1,楊杰1,梁光焰2,王道平2,楊俊*1

                (1. 遵義醫藥高等??茖W校 藥學系,貴州 遵義  563006;2. 貴州省中國科學院天然產物化學重點實驗室,貴州 貴陽  550014)

                 

                摘要3種羥基喹唑啉-4-酮為原料,經乙?;?、氯化、取代、水解、烷基化反應得到6個末端含有端炔取代的4-苯胺喹唑啉類化合物,同時以5-氟尿嘧啶為原料,經羰基保護、烷基化、疊氮化反應制得1-(3-疊氮丙基)-5-氟尿嘧啶,最后再利用藥物拼合原理將其與不同含有端炔取代的4-苯胺喹唑啉類化合物或厄洛替尼通過Click反應合成了75-氟尿嘧啶與4-苯胺喹唑啉骨架的新型拼接產物,其結構通過1HNMRHRMS確證。以厄洛替尼為陽性對照,采用MTT法初步評價目標化合物對人肝癌細胞HepG2、人非小細胞肺癌細胞A549、人宮頸癌細胞Hela、人乳腺癌細胞MCF-7、人肺腺癌耐順鉑株細胞A549/DDP的抑制作用,同時采用ELISA法檢測目標產物對EGFR的抑制能力。結果顯示,1-(3-(4-(((4-((4-碘苯基)氨基)-7-甲氧基喹唑啉-6-))甲基)-1H-1,2,3-三唑-1-)丙基)-5-氟尿嘧啶-2,4(1H,3H)-二酮對HepG2、A549、A549/DDP細胞的抑制作用分別是陽性對照厄洛替尼的6.5倍、1.8倍、2.8倍,對Hela、MCF-7細胞的IC50也分別達到了(0.95 ± 0.33μmol/L,(1.26 ± 0.55 μmol/L。同時,該化合物0.01、0.1 μmol/LEGFR的抑制作用弱于陽性對照厄洛替尼,提示該化合物并非只通過作用于EGFR產生抗腫瘤作用,可能還存在的其他作用途徑,值得進一步研究。

                關鍵詞5-氟尿嘧啶;喹唑啉;Click反應;抗腫瘤;表皮生長因子

                中圖分類號:R914       文獻標識碼:A         文章編號:0258-32832022--

                 

                Synthesis and Antitumor Activity of 5-Fluorouracil and 4-Anilinoquinazoline Skeleton Based on Click Approach LIANG Guang-ping1, YANG Jie1, LIANG Guang-yan2, WANG Dao-ping2, YANG Jun*1 (1. Department of Pharmacy, Zunyi Medical and Pharmaceutical College, Zunyi 563006, China; 2. The Key Laboratory of Chemistry for Natural Products of Guizhou Province and Chinese Academy of Sciences, Guiyang 550014, China), Huaxue Shiji, 2022, 449

                AbstractHydantoin is a class of five-membered heterocyclic compound with four functional points, showing various amazing biological and pharmacological activities. This small and rigid backbone could effectively act on various pharmacological targets. Several clinically important medicines such as phenytoin (antiepileptic), azimilide (antiarrhythmic) and nilutamide (antiandrogen) are based upon this characteristic staple scaffold. RU58841(IUPAC name: 4[3(4hydroxybutyl)4,4dimethyl2,5dioxoimidazolidin1yl]2(trifluoromethyl)benz onitrile) was found active against baldness with little evidence of toxicity, showing a good promise as a topically new active non-steroidal antiandrogen. In this work, we develop a new alternative strategy for synthesis of RU58841 by using 4-amino-2-(trifluoromethyl) benzonitrile as a raw material in four steps including the preparation of isocyanate, [3+2] cycloaddition, N-alkylation and deprotection with over-all yield of 40%. Compare to traditional methods for preparation of RU58841, the strategy in this work is more convenient and safer.

                Key words5-fluorouracil; quinazoline; Click reaction; antitumor; EGFR

                引用本文:梁光平, 楊杰, 梁光焰, . 基于Click反應的5-氟尿嘧啶與4-苯胺喹唑啉骨架的拼接合成及其抗腫瘤活性評價[J]. 化學試劑, 2022, 44(9):1272-1279.

                 

                 

                基于靛紅酸酐-苯并噻唑的Hg2+可視化熒光探針的合成及性能研究

                趙小麗,吳林利,楊迪,冷艷麗,李小紅*,蔡小華*

                貴州民族大學 化學工程學院,貴州 貴陽  550025

                 

                摘要Hg2+由于易生物積累和高毒性的特點,會對人體健康和環境帶來嚴重的危害,因此開發Hg2+簡便、快速、選擇性好、靈敏度高的檢測方法非常重要。通過一步水熱法合成2-氨基-N-(苯并噻唑基)苯甲酰胺,在含水體系V(DMSO)V(H2O) = 1:1快速檢測Hg2+,Hg2+加入后,熒光顯著猝滅。且檢測時不受Ca2+、Hg2+、Mn2+、Cd2+、Co2+、Mg2+、Al3+、Ag+、Zn2+、Ni2+、Fe3+、Cu2+Pb2+的干擾,具有良好的專一選擇性。同時,研究了該熒光探針檢測Hg2+的試紙實驗,發現在熒光探針溶液濃度為2×10-4 mol/L時,可以明顯的檢測出Hg2+。表明該探針對食品和環境中Hg2+的檢測中具有潛在的應用前景。

                關鍵詞:熒光探針;Hg2+;選擇性;靛紅酸酐;2-氨基苯并噻唑

                中圖分類號:O657.3  文獻標識碼:A     文章編號:0258-32832022

                 

                Study and Synthesis of Hg2+ Visible Fluorescent Probe Based on Indigo Anhydride-benzothiazole ZHAO Xiao-li, WU Lin-li, YANG Di, LENG Yan-li, LI Xiao-hong*, CAI Xiao-hua* (Guizhou Minzu University, Guiyang 550025), HuaxueShiji, 2022

                Abstract: Mercury (Hg2+) in aquatic ecosystems is always an important issue because it is one of the most prevalent and dangerous pollutants, with the character of easy bioaccumulation and high toxicity.So it is very important to develop a simple, rapid, selective and sensitive detection method for Hg2+.In this study, we reported a novel fluorescent probe synthesized by one-step hydrothermal method for visual detection of Hg2+ based on a chromogenic reaction under ultraviolet light. It can quickly detect Hg2+ in aqueous system (V(DMSO):V(H2O) = 1:1)with the significant quenching of fluorescence intensity. In addition, the compound 1 can be used to effectively and selectively detect Hg2+ions over other metal ions with a good linear response. At the same time, the test paper experiment of detecting Hg2+ with this fluorescent probe was studied, and it was found that when the concentration of fluorescent probe solution was 2×10-4 mol/L, Hg2+ could be detected obviously.It shows that the probe has a potential application prospect in the detection of Hg2+ in food and environment.

                Key words: fluorescence probe; Hg2+; selectivity; indigo anhydride; 2-aminobenzothiazole

                引用本文趙小麗,吳林利,楊迪,.基于靛紅酸酐-苯并噻唑的Hg2+可視化熒光探針的合成及性能研究[J].化學試劑, 2022,44(9): 1280-1286.

                 

                 

                氨基修飾的N-O功能化金屬有機框架材料的發光性能

                 

                張文謙*,牛亞杰,曹鐸

                信陽農林學院 制藥工程學院,河南 信陽  464000

                 

                摘要熒光類的金屬有機框架(MOFs)因其突出的光學特性、永久孔隙率、可調控的結構和相對較長的發射波長,成為一種具有廣闊應用前景的新型傳感材料。采用協同策略,將軸手性2,2'-聯吡啶-3,3'-二羧酸-1,1'-二氧(H2dpdcdo)含氧配體和氨基修飾的N2-(吡啶-2-)吡啶-2,6-二胺(pda)含氮配體,通過擴散法與Zn(OAc)2·2H2O金屬鹽合成了一種新型熒光MOF材料{[Zn(dpdcdo)(pda)]·H2O·0.5DMF}n。通過單晶X射線衍射(SCXRD)、粉末X射線衍射(PXRD)、紅外光譜(IR)、元素分析(EA)、熱重分析(TGA熒光光譜對MOF {[Zn(dpdcdo)(pda)]·H2O·0.5DMF}n進行了表征。材料{[Zn(dpdcdo)(pda)]·H2O·0.5DMF}nRS-dpdcdo配體連接Zn1pda分別產生一維左手鏈和右手鏈,兩種手性鏈之間通過氫鍵作用和π-π堆積作用形成了三維外消旋結構。固態熒光測試顯示,MOF {[Zn(dpdcdo)(pda)]·H2O·0.5DMF}n相比于配體,發射峰出現了大幅度紅移,在523 nm處有一強發射峰,在紫外燈照射下發出明顯的黃綠色熒光。離子識別實驗表明MOF 材料{[Zn(dpdcdo)(pda)]·H2O·0.5DMF}n是一種檢測MnO4-離子的良好熒光探針。

                關鍵詞熒光金屬有機框架;熒光傳感;熒光淬滅;離子識別

                中圖分類號:O61    文獻標識碼:A      文章編號:0258-32832022

                 

                Fluorescent Properties of Amino-Decorated N-Oxide Functional Metal-Organic Framework ZHANG Wen-qian*, NIU Ya-jie, CAO Duo. (College of Pharmaceutical Engineering, Xinyang Agricultural and Forestry University, Xinyang 464000, China), Huaxue Shiji, 2022,

                AbstractFluorescent metal-organic frameworks (MOFs) have become a new sensing material with broad application prospects because of their outstanding optical properties, permanent porosity, adjustable structures and relatively long emission wavelength. A novel fluorescent MOF, {[Zn(dpdcdo)(pda)]·H2O·0.5DMF}n, was synthesized by synergistical combination of diffusion method with axial chirality 2,2'-bipyridine-3,3'-dicarboxylic acid-1,1'-dioxygen (H2dpdcdo) as oxygenated ligand, amino-decorated N2-(pyridin-2-yl) pyridine-2,6-diamine (pda) as nitrogenous ligand, and Zn(OAc)2·2H2O as metal salt. The obtained MOF was characterized by single-crystal X-ray diffraction (SCXRD), powder X-ray diffraction (PXRD), infrared spectroscopy (IR), elemental analysis (EA), thermogravimetric analysis (TGA) and fluorescent spectroscopy. In MOF {[Zn(dpdcdo)(pda)]·H2O·0.5DMF}n, R and S-dpdcdo ligands connect with Zn1 and pda to produce one-dimensional left-handed chains and right-handed chains, respectively. And then, they are extended by hydrogen bonding and π-π stacking interactions to form a three-dimensional racemic structure. The solid-state fluorescence tests show that compared with the ligands, the emission peak of as-prepared MOF exhibits a significant red shift at 523 nm, which corresponds to obvious yellow-green fluorescence under the irradiation of UV lamp. Anion recognition tests demonstrate that MOF {[Zn(dpdcdo)(pda)]·H2O·0.5DMF}n is an efficient fluorescent probe for detection of MnO4- ion.

                Key wordsfluorescent metal-organic framework; fluorescence sensing; fluorescence quenching; ion recognition

                引用本文:張文謙, 牛亞杰, 曹鐸. 氨基修飾的N-O功能化金屬有機框架材料的發光性能[J]. 化學試劑, 2022,4491287-1293.

                 

                 

                一個單核鈷(Ⅱ)超分子配合物的合成、晶體結構及類Fenton催化性質研究

                張倩*a,葉英杰a,于瓊燕b,陳壘a

                河南工程學院  a.化工與印染工程學院,b.材料工程學院,河南 鄭州  450007

                 

                摘要合成得到了一個配體1,3-二羧甲基苯并咪唑,將其與Co(Ac)2·4H2O在水溶液中反應得到了一個新的單核鈷(II)配合物,并通過X-射線單晶衍射和元素分析表征了其晶體結構。配合物為一個金屬中心與2個配體和4個水分子形成單核結構,單核結構之間再通過O—H···H氫鍵及π···π堆積作用組裝成三維超分子網絡結構。并測試了此配合物的物相純度、熱穩定性質和作為非均相類Fenton試劑的催化性質,測試結果表明,配合物顯示了良好的物相純度,對甲基橙溶液可以達到86.0%的降解率,顯示了良好的類Fenton催化性質,表明是一種潛在的催化降解有機污染物的材料。

                關鍵詞:(Ⅱ)超分子配合物;晶體工程;苯并咪唑二羧酸;類Fenton試劑;甲基橙降解

                中圖分類號:O614     文獻標識碼:A      文章編號:0258-32832022--

                 

                Synthesis, crystal structure and Fenton-like catalytic property of a Cobalt(II) mononuclear supramolecular complex ZHANG Qian*1, YE Ying-jie1, YU Qiong-yan2 , CHEN Lei1 (1.College of Chemical and Printing-dyeing Engineering, Henan University of Engineering, Zhengzhou 450007, Henan; College of Materials Engineering, Henan University of Engineering, Zhengzhou 450007, Henan), Huaxue Shiji, 2022, 44(9),

                Abstract: Mercury (Hg2+) in aquatic ecosystems is always an important issue because it is one of the most prevalent and dangerous pollutants, with the character of easy bioaccumulation and high toxicity. So it is very important to develop simple, rapid, selective and sensitive detection methods for Hg2+. In this study, we reported a novel fluorescent probe synthesized by one-step hydrothermal method for visual detection of Hg2+ based on a chromogenic reaction under ultraviolet light. Hg2+ can be quickly detected in aqueous system (V(DMSO) : V(H2O) = 1:1) on the basis of the significant quenching of fluorescence intensity. In addition, the compound 1 can be used to effectively and selectively detect Hg2+ ions over other metal ions (Ca2+、Hg2+、Mn2+、Cd2+、Co2+、Mg2+、Al3+、Ag+、Zn2+、Ni2+、Fe3+、Cu2+ and Pb2) with a good linear response. Furthermore, the test paper experiment of detecting Hg2+ by this fluorescent probe was studied, and it was found that when the concentration of fluorescent probe solution was 2×10-4 mol/L, Hg2+ could be distinguished obviously. Such probe shows a good potential for the detection of Hg2+ in food and environment.

                Key words: Co(II) supramolecular complex; crystal engineering; benzimidazolyl dicarboxylic acid; Fenton-like agent; MO degradation

                引用本文:張倩,葉英杰,于瓊燕,等. 一個單核鈷(Ⅱ)超分子配合物的合成、晶體結構及類Fenton催化性質研究[J]. 化學試劑,2022,44(9): 1294-1298。

                 

                 

                脫脂油茶籽粕多糖的提取及抗氧化活性研究

                林莉*1,石慶楠2,周敏1,楊衛林3,龍開偉3,羅麗君1

                1. 凱里學院 大健康學院,貴州 凱里  556001;2. 黔東南州食品藥品檢驗檢測中心,貴州 凱里  556000;3. 貴州綠色農業開發有限公司,貴州 錦屏  556704

                 

                摘要研究水提醇沉法提取多糖的工藝并測定其體外抗氧化活性,以期為提高油茶副產物資源的利用率提供理論依據。以脫脂油茶籽粕為原料,采用水提醇沉法在單因素試驗基礎上結合響應面法對多糖提取工藝優化,并通過測定DPPH自由基、O2-自由基、·OH自由基分析其體外抗氧化活性。脫脂油茶籽粕多糖提取的最佳工藝參數為VV=130 g/mL、提取溫度80 ℃、提取時間50 min,在此工藝參數下脫脂油茶籽粕多糖提取率為49.25%,RSD0.24%;清除DPPH自由基、O2-自由基、·OH自由基的半抑制濃度(IC50)分別為1.67、1.44、1.94 mg/mL。響應面試驗建立的優化模型對脫脂油茶籽粕多糖提取率分析可靠且所得多糖具有一定的體外抗氧化效果。

                關鍵詞脫脂油茶籽粕;多糖;響應面;提??;抗氧化活性

                中圖分類號:TS202.1       文獻標識碼:A      文章編號:0258-32832022--

                 

                Study on extraction and antioxidant activity of polysaccharide from degreased camellia LIN Li*1, SHI Qing-nan2, ZHOU Min1, YANG Wei-lin3, LONG Kai-wei3, LUO Li-jun11.School of Life and Health Science, Kaili college, Kaili 556001, China; 2. Qiandongnan Food and Drug Inspection and Testing Center, Kaili  556001, China; 3. Guizhou Green Agriculture Development Co. Ltd, Jinpin 556704, China, Huaxue Shiji, 2022, 44(9),

                Abstract: In the purpose of providing theoretical basis for improving the utilization rate of camellia byproduct resources, we study the extraction technology of polysaccharide by water extraction and alcohol precipitation method, and evaluate its antioxidant activity in vitro. By employing degreased camellia as a raw material, and optimizing the extraction process of polysaccharide through water extraction and alcohol precipitation method on the basis of single factor test and response surface methodology, the antioxidant activity of polysaccharides was then evaluated by DPPH, O2- and ·OH radicals. The optimal extraction conditions were demonstrated to be solid-liquid ratio of 1 : 30 g/mL, temperature of 80 and time of 50 min. Under these conditions, the extraction rate and RSD of polysaccharides was determined to be 46.12% and 0.24%, respectively. Meanwhile, the scavenging concentrations (IC50) for DPPH, O2- and ·OH radicals were 1.67, 1.44 and 1.94 mg/mL. The optimized model established by response surface test was reliable for the extraction rate analysis of polysaccharides from defatted camellia, and the obtained polysaccharides showed good antioxidant activity in vitro.

                Key words: Degreased camellia;polysaccharide;responsesurface;extraction;antioxidantactivity

                引用本文:林莉,石慶楠,周敏,等. 脫脂油茶籽粕多糖的提取及抗氧化活性研究[J]. 化學試劑,2022,44(9): 1299-1305。

                 

                 

                鋁離子電池正極材料的研究進展

                 

                譚斌1,羅文斌*2,晁自勝*2

                1.湖南鐵道職業技術學院,湖南 株洲 412001;

                2.長沙理工大學 材料科學與工程學院,湖南 長沙 410114

                 

                摘要:Al價格低且儲量在地殼中儲量較為豐富,體積比容量最高,電化學當量和質量比容量僅分別略高于和低于Li,因此,鋁離子電池具有非常廣闊的發展前景。然而,鋁離子電池正極材料尚存在著一些問題循環穩定性強但放電比容量低放電比容量高容量衰減嚴重。此外,充放電反應機理上也存在分歧,這些問題的存在限制了高能量密度鋁離子電池的進一步發展。結合前人相關研究,總結了離子電池正極材料的研究現狀和優化方法,并對相關問題進行了分析與展望。

                關鍵詞:鋁離子電池;正極材料;金屬硫化物;金屬氧化物;碳材料

                中圖分類號:TM912       文章標識碼:A       文章編號0258-32832022

                 

                Research Progress of Cathode Materials for Aluminum Ion Batteries TAN Bin1, LUO Wen-bin*2, CHAO Zi-sheng*2 (1. Hunan Railway Professional Technology College, Zhuzhou 412001, China; 2. College of Materials Science and Engineering,Changsha University of Science and Technology, Changsha 410114, China), Huaxue Shiji, 2022,449

                Abstract: Due to its low price, richest reserve in the crust and highest volume specific capacity of Al, along with its electrochemical equivalent and mass specific capacity are only slightly higher and lower than Li, therefore aluminum-ion batteries (AIBs) have a very broad application potential. Nevertheless, there are still some problems in the cathode materials of aluminum-ion batteries, such as strong cycle stability but low discharge capacity, or high discharge capacity rather than serious capacity fading. In addition, there are controversies in the charge-discharge reaction mechanisms, limiting the further development of high energy density aluminum ion batteries. In this review, the research status of cathode materials was summarized based on previous research and theories, and the current related problems and perspectives were discussed as well.

                Key words: aluminum ion batteries; cathode materials; metal sulfide; metal oxide; carbon material

                引用本文:譚斌,羅文斌,晁自勝. 鋁離子電池正極材料的研究進展[J].化學試劑,2022,449:1306-1313.

                 

                 

                虛擬模板分子印跡材料固相萃取磺胺類抗生素

                王藝曉1,4,孫宏宵1,2a,王莉燕1,4,紀靈*3,孫大妮1,2c,劉惠濤2c,宋志花2b,李金花*1,4

                 

                1. 中國科學院煙臺海岸帶研究所 山東省海岸帶環境工程技術研究中心 中國科學院海岸帶環境過程與生態修復重點實驗室 山東省海岸帶環境過程重點實驗室,山東 煙臺  264003;2. 煙臺大學 a. 環境與材料工程學院,b.藥學院 分子藥理和藥物評價教育部重點實驗室 新型制劑與生物技術藥物研究山東省高校協同創新中心,c.化學化工學院,山東 煙臺  264005;3. 國家海洋局煙臺海洋環境監測中心站,山東 煙臺  264006;4. 中國科學院大學,北京  100049

                   

                  摘要以磺胺苯(SZ)為虛擬模板,一步沉淀聚合制備虛擬模板分子印跡聚合物(DMIPs)材料,用于同時分散固相萃?。?/span>DSPE)水樣中4種磺胺類抗生素(SAs),結合HPLC-UV進行測定。對DMIPs進行表征與吸附性能評價,其對4SAs的最大吸附量為21.9730.24 mg/g,印跡因子均大于2.1。優化DMIPs用量、萃取時間、樣品溶液pH等,確定最佳DSPEHPLC條件。在湖水、海水、自來水中評價方法的分析性能,得到3種水樣中的線性范圍為1200 μg/L、檢出限0.270.64 μg/L和定量限0.992.14 μg/L?;|效應結果(ME%6%)表明DMIPs-DSPE有效消除了復雜基質干擾、提高了檢測準確度。4SAs3中水樣中的回收率為93.8%102.6%,相對標準偏差(RSD)為2.6%7.0%。該DMIPs-DSPE-HPLC-UV法簡單快速、靈敏準確,適于復雜樣品中痕量SAs多殘留分析。

                  關鍵詞磺胺類抗生素;分子印跡聚合物;虛擬模板;固相萃取;環境水樣; 高效液相色譜

                  中圖分類號:O615.4     文獻標識碼:A       文章編號:0258-32832022

                   

                  Solid-phase Extraction of Sulfonamides Antibiotics by Using Dummy Template Based Molecularly Imprinted Materials WANG Yi-xiao1,4, SUN Hong-xiao1,2a, WANG Li-yan1,4, JI Ling*3, SUN Da-ni12c, LIU Hui-tao2c, SONG Zhi-hua2b, LI Jin-hua*1,41.CAS Key Laboratory of Coastal Environmental Processes and Ecological Remediation, Shandong Key Laboratory of Coastal Environmental Processes, Shandong Research Center for Coastal Environmental Engineering and Technology, Yantai Institute of Coastal Zone Research, Chinese Academy of Sciences, Yantai 264003, China; 2. a. School of Environmental and Material Engineering;b.School of Pharmacy, Collaborative Innovation Center of Advanced Drug Delivery System and Biotech Drugs in Universities of Shandong, Key Laboratory of Molecular Pharmacology and Drug Evaluation (Yantai University), Ministry of Education,c. College of Chemistry and Chemical Engineering, Yantai University, Yantai 264005, China; 3. Yantai Oceanic Environmental Monitoring Central Station, State Oceanic Administration, Yantai 264006, China; 4. University of Chinese Academy of Sciences, Beijing 100049, China)

                  AbstractIn this work, dummy template molecularly imprinted polymers (DMIPs) were prepared by one-step precipitation polymerization using sulfameobenzene (SZ) as a dummy template, and applied for the simultaneous dispersion of four typical SAs in solid-phase extraction (DSPE), followed by high performance liquid chromatography-UV (HPLC-UV) determination. The DMIPs was characterized by several techniques, such as SEM and FT-IR, and its static/dynamic adsorption and selectivity were all evaluated by using adsorption models. The maxima adsorption capacities of sulfamonomethoxine (SMM), sulfachloropyridazine (SFZ), sulfamethoxazole (SMX) and sulfadimethoxine (SDM) were 30.24, 28.61, 21.97 and 22.37 mg/g, respectively, and the imprinting factors were all greater than 2.1. The factors affecting the extraction efficiency of DMIPs-DSPE, mainly including dosage of DMIPs, extraction time, pH of sample solution, volume of desorption and time of desorption were systematically optimized. Under the optimal conditions, the DMIPs-DSPE-HPLC-UV methods attained good linearity in the range of 1200 μg/L with correlation coefficients 0.9995, and the limits of detection (LODs) were between 0.270.64 μg/L and the limits of quantification (LOQs) were 0.992.14 μg/L in lake water, seawater and tap water samples. The precision of the method was excellent, for example, the intraday precision (relative standard deviation, RSD) of retention time and peak area of the four SAs were 0.07%0.12% and 0.53%1.13%, respectively, and the interday precision was 0.23%0.28% and 0.95%1.33%, respectively. The matrix effect (ME) of the method was investigated to be ME 6% in the above three water samples, indicating that the developed method can effectively eliminate the interference of complex matrices. The recoveries of four SAs in lake water, seawater, tap water were 93.8%99.8%, 94.8%100.1% and 95.6%102.6%, respectively, with RSD of 2.6%7.0%, 2.8%5.4% and 2.8%5.2%. The simple, rapid, sensitive and accurate DMIPs-DSPE-HPLC-UV method proved applicable for multiresidue analysis of SAs in complicated samples.

                  Key wordssulfonamides antibiotics;molecularly imprinted polymers;dummy template;solid-phase extraction;environmental water samples;high performance liquid chromatography

                引用本文:王藝曉,孫宏宵,王莉燕,等.虛擬模板分子印跡材料固相萃取磺胺類抗生素[J].化學試劑,2022,4491314-1324.

                 

                 

                汞離子熒光探針的研究進展

                張人杰,史紀福,王雪,馮貞,劉姝菂*

                煙臺大學 化學化工學院,山東 煙臺  264005

                 

                摘要汞是一種具有生物積累性的重金屬元素,與一系列疾病的發生發展有密切聯系。為了實現汞離子的實時原位可視化檢測,近年來檢測汞離子的有機小分子熒光探針發展迅速并有相關綜述報道,但對于高分子熒光材料檢測汞離子的研究報道極少。與其他汞離子研究進展綜述不同之處在于以汞離子的檢測機理為出發點,分別從設計原理、選擇性、靈敏度和實用性角度綜述,簡要介紹了近年來有機小分子探針的設計策略,詳細介紹了基于功能高分子熒光材料檢測汞離子的研究進展,將其檢測策略歸納為配位型、反應型及兩者結合型三類,以期為汞離子熒光探針的設計及發展提出新的研究思路。

                關鍵詞:熒光探針;汞離子;高分子熒光材料;檢測機理;配位作用

                中圖分類號:O614.24         文獻標識碼:A    文章編號:0258-32832022

                 

                Recent Progress in Mercury Ions Fluorescent Probes ZHANG Ren-jie, SHI Ji-fu, WANG Xue, FENG Zhen, LIU Shudi* (College of Chemistry and Chemical Engneering, Yantai University, Yantai  264005, China) , Huaxue Shiji,2022,44 (9),00 ~ 00

                AbstractMercury is a heavy metal element closely related to the occurrence and development of a series of diseases on account of its bioaccumulation. In order to realize the in situ and real-time visual detection of mercury ions, small organic molecules based fluorescent probes for mercury ions have been developed rapidly in recent years and these related works have been summarized and reported as review papers, but the mercury ion probes fabricated using polymer fluorescent materials have been rare reviewed. The difference between this review and others is that the research progress of small organic molecule based mercury ions fluorescent probes was first briefly introduced and then highlights the advances in mercury ions detection using functional fluorescent polymer materials in recent years, including design principle, selectivity, sensitivity and practicality. The detection strategies were classified into three types, including coordination type, reaction-based type and combination type based on aspects of response mechanism strategy. This review would be helpful to design and develop ideal fluorescent probes for mercury ions detection. 

                Key wordsfluorescent probe; mercury ions; polymer fluorescent materials; detection mechanism; coordination

                引用本文:張人杰,史紀福,王雪,等.汞離子熒光探針的研究進展[J]. 化學試劑,2022,44(9): 1325-1333。

                 

                 

                喹諾酮類抗生素的分子印跡電化學傳感檢測

                溫宇浩1,3,孫大妮2,3,張悅3,周娜3,劉惠濤2,李金花*1,3,莊旭明*2

                1. 哈爾濱工業大學(威海)  海洋科學與技術學院,山東 威海  264209;2.煙臺大學 化學化工學院,山東 煙臺  264005;3.中國科學院煙臺海岸帶研究所 山東省海岸帶環境工程技術研究中心 中國科學院海岸帶環境過程與生態修復重點實驗室 山東省海岸帶環境過程重點實驗室,山東 煙臺  264003)

                   

                  摘要喹諾酮類抗生素(QNs)殘留極大危害生物體和環境,其含量低、種類多、基質復雜,通常需要進行樣品前處理結合色譜/質譜分析以實現靈敏檢測。分子印跡聚合物(MIPs)是具有與模板分子在形狀、大小及官能團完全匹配的特異性識別位點的高分子聚合物,能選擇性識別和富集目標分析物并消除干擾。電化學傳感器具有高靈敏度、高選擇性、響應時間短等優點,將分子印跡技術應用其中,得到的分子印跡電化學傳感器(MIEC)具備了二者的優點。綜述了MIEC的構建原理,主要包括電流傳感器和電位傳感器。此外,重點介紹了MIEC在工業生產和實際生活中對QNs的檢測,包括恩諾沙星、氧氟沙星等。最后,提出了MIECQNs快速檢測中面臨的挑戰和發展前景。

                  關鍵詞喹諾酮類抗生素;分子印跡聚合物;電化學傳感器;構建原理;快速檢測

                  中圖分類號:O657.1    文獻標識碼:A        文章編號: 

                   

                  Molecular Imprinting based Electrochemical Detection of Quinolones Antibiotics WEN Yu-hao1,3, SUN Da-ni2,3, ZHANG Yue3, ZHOU Na3, LIU Hui-tao2, LI Jin-hua*1,3, ZHUANG Xu-ming*2 (1. School of Marine Science and Technology, Harbin Institute of Technology (Weihai), Weihai 264209, China; 2. College of Chemistry and Chemical Engineering, Yantai University, Yantai 264005, China; 3. CAS Key Laboratory of Coastal Environmental Processes and Ecological Remediation, Shandong Key Laboratory of Coastal Environmental Processes, Shandong Research Center for Coastal Environmental Engineering and Technology, Yantai Institute of Coastal Zone Research, Chinese Academy of Sciences, Yantai 264003, China)

                  Abstract: The residues of quinolones (QNs) antibiotics are extremely harmful to organisms and the environment. QNs are low in content and diverse in species, and present in complex matrices. Usually, sample pretreatment combined with chromatographic/mass spectrometry analysis is required to achieve sensitive detection. Molecularly imprinted polymers (MIPs) are high molecular polymers with specific recognition sites that exactly match template molecules in shape, size and functional groups, which can selectively recognize and enrich target analytes and eliminate interference. Electrochemical sensors have the advantages of high sensitivity and selectivity, and short response time. Molecularly imprinted electrochemical sensors (MIES) obtained by applying molecular imprinting technology have the advantages of both MIPs and electrochemical sensors. In this Review, we summarize the construction principles of MIEC, mainly including current sensors and potential sensors. The detection of QNs (enrofloxacin, ofloxacin, etc.) in industrial production and real life by MIES is then highlighted. Finally, the challenges and development prospects of MIEs in rapid detection of QNs are discussed.

                  Key wordsquinolones antibiotics; molecularly imprinted polymers; electrochemical sensors; construction mechanism; rapid detection

                引用本文:溫宇浩,孫大妮,張悅,等.喹諾酮類抗生素的分子印跡電化學傳感檢測[J].化學試劑,2022,4491334-1341.

                 

                 

                環境新污染物風險防范與化學品環境管理

                時巧翠1,傅佳宇2,陳金媛*2,周宇暢1

                1.浙江警察學院 浙江省毒品防控技術研究重點實驗室,浙江 杭州  310053;

                2. 浙江工業大學 環境學院,浙江 杭州  310014

                 

                摘要:隨著各類化學品的大量使用,環境內分泌干擾物、新型持久性有機污染物、微塑料和抗生素等新污染物對生態環境和人體健康的危害正逐步顯現并日趨嚴重。如何進一步完善我國環境新污染物的風險防范體系,是我國生態環境治理面臨的重要問題?;瘜W品環境管理是防范環境新污染物風險的重要環節。通過查閱文獻資料梳理了我國環境新污染物風險防范和化學品管理的政策法規及相關規定,在此基礎上,結合當前存在的問題,從制度建設、體制機制、監測評估及科學研究等方面提出了建議。

                關鍵詞:環境內分泌干擾物;新型持久性有機污染物;微塑料;抗生素;風險防范;化學品環境管理       

                中圖分類號:X327    文獻標識碼:A     文章編號:0258-32832022

                 

                Risk Prevention of Emerging Pollutants and Environmental Management of Chemicals SHI Qiao-cui 1, FU Jia-yu 2, CHEN Jin-yuan *2, ZHOU Yu-chang1 (1.Laboratory of Drug Prevention and Control Technology of Zhejiang Province, Zhejiang Police College Hangzhou 310053,China; 2.College of Environment, Zhejiang University of Technology, Hangzhou 310014,China) , Huaxue Shiji,2022,44 (9)

                Abstract: With the extensive use of various chemicals, the harm of some new emerging pollutants such as environmental endocrine disruptors, new persistent organic pollutions, microplastics and antibiotics to Chinese residents, ecology and environment is gradually appearing, and it is becoming more and more serious. How to further improve the risk prevention system of China’s emerging pollutants is an important issue facing China’s ecological environment governance. Synthetic chemicals and unintentionally released chemical substances constitute an important source of new emerging pollutants. Environmental management of chemicals is very imperative to risk prevention of emerging pollutants. This review summarizes the literatures on Chinas policies, laws and related regulations of risk prevention of emerging pollutants and control of chemicals. And on this basis we put forward the system construction, system and mechanism, evaluation and monitoring, and scientific research suggestions.

                Key wordsenvironmental endocrine disruptors; new persistent organic pollutions; microplastics; antibiotics; risk prevention; environmental management of chemicals

                引用本文:時巧翠,傅佳宇,陳金媛,等. 環境新污染物風險防范與化學品環境管理[J]. 化學試劑,2022,44( 9): 1342-1349。

                 

                 

                分子印跡技術用于抗生素殘留檢測的研究進展

                 

                趙廣麗1,張悅1,孫大妮2,周娜*2,韓鎧營1,閆李霞3,于佳洛2,宋志花1,李桂生*1

                1. 煙臺大學 藥學院 分子藥理和藥物評價教育部重點實驗室 新型制劑與生物技術藥物研究山東省高效協同創新中心,山東 煙臺 264005;2. 中國科學院煙臺海岸帶研究所 中國科學院海岸帶環境過程與生態修復重點實驗室,山東 煙臺 264003;3. 山東省煙臺第二中學,山東 煙臺 264000

                 

                摘要:模擬酶-底物或抗原-抗體特異性結合原理的分子印跡技術(MIT)在目標物識別和檢測中應用廣泛。MIT制備的分子印跡聚合物(MIPs)為吸附劑的分子印跡固相萃?。?/span>MISPE)和基于MIPs的傳感分析均已廣泛應用于抗生素的分析檢測中。簡要介紹了抗生素MIPs的幾種新興制備技術,包括表面印跡、納米印跡、活性可控自由基聚合、多模板印跡、多功能單體印跡和虛擬模板印跡;然后,概述了基于MIPs3種固相萃?。?/span>SPE)模式,即傳統裝柱固相萃取、磁固相萃取、分散固相萃取,以及基于MIPs傳感器的基本原理。隨后,重點綜述了近5MISPE和基于MIPs的電化學和熒光傳感器用于環境和食品等樣品中的各種抗生素殘留檢測的研究進展,包括磺胺類、喹諾酮類、四環素類等。最后,對抗生素MIPs的制備和應用進行了展望。

                關鍵詞:抗生素;印跡技術;分子印跡聚合物;固相萃??;傳感器

                中圖分類號:R917    文獻標識碼:A       文章編號:0258-32832022

                 

                Research Advances of Molecular Imprinting Technology for the Detection of Antibiotics Residues ZHAO Guang-li1, ZHANG Yue1, SUN Da-ni2, ZHOU Na*2, HAN Kai-ying1, YAN Li-xia3, YU Jia-luo2, SONG Zhi-hua1, LI Gui-sheng*1 (1. Key Laboratory of Molecular Pharmacology and Drug Evaluation, Ministry of Education, Shandong Provincial High-efficiency Collaborative Innovation Center for Novel Formulations and Biotechnology Drug Research, School of Pharmacy, Yantai University, Yantai 264005, China; 2. CAS Key Laboratory of Coastal Environmental Processes and Ecological Remediation, Yantai Institute of Coastal Zone Research, Chinese Academy of Sciences, Yantai 264003, China; 3. Yantai No.2 Middle School of Shandong Province, Yantai 264000, China), Huaxue Shiji, 2022,

                Abstract: Molecular imprinting technology (MIT), which mimics the specific binding principle of enzyme-substrate or antigen-antibody, is widely used in target recognition and detection. Molecularly imprinted polymers (MIPs) based sensing assays and molecularly imprinted solid-phase extraction (MISPE) fabricated from MIPs (prepared by MIT) as adsorbents, have been widely applied in the detection of antibiotics. This review briefly introduces several emerging preparation techniques for antibiotics MIPs, including surface imprinting, nanoimprinting, living-controlled radical polymerization, multitemplate imprinting, multifunctional monomer imprinting, and dummy template imprinting. Solid-phase extraction (SPE) modes, namely traditional column-packed SPE, magnetic SPE, dispersive SPE, and the basic principle of MIPs based sensors are outlined. Subsequently, the recent 5-year application advances of MISPE and MIPs-based electrochemical and fluorescence sensors in the detection of various antibiotics residues, such as sulfonamides, quinolones and tetracyclines in environmental, food and other samples are highlighted. Finally, the preparation and application of antibiotics MIPs are prospected.

                Key wordsantibiotics; imprinting technology; molecularly imprinted polymers; solid-phase extraction; sensors

                引用本文趙廣麗, 張悅, 孫大妮, . 分子印跡技術用于抗生素殘留檢測的研究進展[J]. 化學試劑, 2022, 449):1350-1359.

                 

                 

                分子印跡技術在中藥研究中的應用進展

                 

                韓鎧營,張悅,宋志花*,畢毅,楊剛強,李桂生*

                (煙臺大學 藥學院 分子藥理和藥物評價教育部重點實驗室 新型制劑與生物技術藥物研究山東省高校協同創新中心,山東 煙臺  264005

                 

                摘要:目前,在中藥現代化和國際化背景下,中藥的相關研究也進入了發展快車道。中藥研究面臨化學成分多樣、基質復雜、有效成分含量低等挑戰,傳統樣品前處理方法由于所需時間長、選擇性低等問題難以解決上述問題。分子印跡技術(Molecular Imprinting Technology,MIT)制備的分子印跡聚合物(Molecularly Imprinted Polymers,MIPs憑借其高選擇性已在中藥研究領域大顯身手,廣泛用于中藥中有效成分提取、有害成分分析、中藥代謝研究等多個方面??偨Y了2017~2022MIT在中藥研究中的應用進展,展望了MIT在中藥研究中的應用。

                關鍵詞:分子印跡;中藥;富集;提??;檢測;代謝產物

                中圖分類號:R932      文獻標志碼:A    文章編號:0258-32832022

                 

                Recent Progress in Research on Traditional Chinese Medicine Based on Molecular Imprinting Technology HAN Kai-ying, ZHANG Yue, SONG Zhi-hua*, BI Yi, YANG Gang-qiang, LI Gui-sheng* (School of Pharmacy,Key Laboratory of Molecular Pharmacology and Drug EvaluationMinistry of Education, Collaborative Innovation Center of Advanced Drug Delivery System and Biotech Drugs in Universities of Shandong, Yantai University, Yantai 264005, China), Huaxue Shiji, 2022,

                AbstractAt present, under the background of modernization and internationalization of traditional Chinese medicine (TCM), the related research of TCM has entered the fast track of development. TCM research is faced with the challenges of diverse chemical components, complex matrix and low content of active components, which are difficult to be solved by traditional sample pretreatment methods due to long waiting time and insufficient selectivity. With their high selectivity, molecularly imprinted polymers (MIPs) prepared by molecular imprinting technology (MIT) have been widely used in the field of TCM research. It is widely used in the extraction of active components, analysis of harmful components and metabolism of traditional Chinese medicine. In this review, the application progress of MIT in TCM from 2017 to 2022 was summarized, and the perspectives on this research field were finally discussed as well.

                Key words: molecular imprinting technology; traditional Chinese medicine; ingredient enrichment; ingredient extraction; pesticide detection; metabolites

                引用本文:韓鎧營, 張悅, 宋志花, . 分子印跡技術在中藥研究中的應用進展[J]. 化學試劑, 2022, 4491360-1367.

                 

                 

                LC-MS方法分析皮膚表面鞘脂的組成

                佟薇1,江芝婷2,胡坪1,章弘揚*1

                (1. 華東理工大學 化學與分子工程學院 上海市功能性材料化學重點實驗室,上海  200237;2. 巴斯夫新材料有限公司 個人護理品部,上海  200137)

                摘要鞘脂作為角質層中最豐富的脂質,在皮膚屏障中起到重要作用。通過建立一種基于超高效液相色譜-四極桿-飛行時間質譜(UPLC-Q-TOF-MS)的分析方法,利用自建數據庫匹配和二級質譜結構解析,對女性皮膚表面的108個鞘脂進行了鑒定并歸納其碎裂機理,其中包括34個鞘氨醇堿、65個神經酰胺(Cer)、81-磷酸神經酰胺(CerP)和1個磷酰鞘脂(PN-Cer)。隨后將該方法應用于青、中年女性前臂皮膚鞘脂的檢測,結合多元變量統計分析,初步探索了皮膚老化的鞘脂代謝差異。結果表明,不同年齡女性皮膚的鞘脂輪廓表現出明顯的分組趨勢,并篩選得到43個差異性鞘脂標志物,這些標志物相對含量的變化可能與衰老皮膚細胞中酶活性的變化有關。本研究為皮膚鞘脂的全面分析提供了新方法,也對皮膚衰老機制的探索及相關抗衰老護膚品的研發,具有一定的理論指導意義。

                關鍵詞皮膚表面鞘脂;UPLC-Q-TOF-MS;多元變量統計分析;皮膚老化;差異性標志物

                中圖分類號:O657.6    文獻標識碼:A      文章編號:0258-32832022 

                 

                Identification of Sphingolipid Compositions in the Skin of Young and Middle-aged Women by LC-MS TONG Wei1, JIANG Zhi-ting2, HU Ping1, ZHANG Hong-yang*1 (1. Shanghai Key Laboratory of Functional Materials Chemistry, School of Chemistry and Molecular Engineering, East China University of Science and Technology, Shanghai 200237, China; 2. Personal Care Department, BASF New Materials Co., Ltd., Shanghai 200137, China), Huaxue Shiji, 2022, 44(9)

                AbstractSphingolipids, as the most abundant lipids in the stratum corneum, play an important role in skin barrier. In this paper, an analytical method based on ultra-high performance liquid chromatography-quadrupole-time-of-flight mass spectrometry (UPLC-Q-TOF-MS) was established to analyze the sphingolipids in women skin surface. By using personal database matching and MS/MS structural analysis, 108 sphingolipids were identified in the skin of women, including 34 of sphingosine bases, 65 of ceramides (Cer), 8 of ceramide 1-phosphates (CerP), and 1 of phosphonosphingolipid (PN-Cer). After then, this method combined with multivariate statistical analysis was applied to detect the metabolic perturbations of sphingolipids associated with skin aging in the young and middle-aged women forearm. The results showed that the skin sphingolipid profiles of young and middle-aged women exhibiting an obvious grouping trend, and 43 of differentiated sphingolipid markers were screened, which might be related to the changes of enzyme activities in aging skin cells. This study could provide a new method for the comprehensive analysis of skin surface sphingolipids, and it also has certain theoretical guiding significance for the exploration of skin aging mechanism and the research and development of related anti-aging skin care products.

                Key wordsskin surface sphingolipids; UPLC-Q-TOF-MS; multivariate statistical analysis; skin aging; differential markers

                引用本文:佟薇,江芝婷,胡坪,等. LC-MS方法分析皮膚表面鞘脂的組成[J]. 化學試劑, 2022, 44(9): 1368-1375。

                 

                 

                穩定性同位素分析在毒品溯源中的應用研究進展

                 

                趙志東1,2,3,孟嬌1,鞏京慧1,王曉卉1,張顯強*1

                1.貴州警察學院,貴州 貴陽  550005;2.中國科學院廣州化學所,廣東 廣州  510650;3.中國科學院大學,北京  100000

                 

                摘要:綜述了穩定性同位素技術在毒品來源推斷中的應用研究進展,包括大麻、可卡因、海洛因、甲基苯丙胺和MDMA。通過對不同來源地毒品樣品的同位素數據以及不同合成路徑和反應條件下反應物和產物的同位素特征進行收集整理并進行深入剖析和挖掘,可以建立毒品樣品與種植地、合成路徑、工藝和反應條件的聯系,進而實現毒品種植地或產地的推斷。穩定性同位素分析數據對于毒品溯源追蹤具有借鑒意義和參考價值。

                關鍵詞:法庭科學;穩定性同位素;毒品;溯源;合成路徑;種植地

                中圖分類號:O65      文獻標識碼:A      文章編號:0258-32832022--

                 

                Research progress on the application of stable isotope analysis in illegal drug traceability ZHAO Zhi-dong1,2,3, MENG Jiao1, GONG Jing-hui1, WANG Xiao-hui1, ZHANG Xian-qiang* 1 (1.Guizhou Police College, Guiyang 550005; 2.Guangzhou Institute of Chemistry, Chinese Academic of Science, Guangzhou  510650; 3.University of Chinese Academic of Science, Beijing 100000,China), Huaxue Shiji, 2022, 449

                Abstract: In this Review, we summarized the application progress of stable isotope technology in tracing the source of drugs, including marijuana, cocaine, heroin, methamphetamine and MDMA. Links of growth location, along with synthetic routes, processes and reaction conditions of drug samples were established by collecting and sorting out. The obtained isotopic data of drug samples from different origins, the isotopic characteristics of reactants and products under different synthetic routes and reaction conditions, was then thoroughly analyzed and studied to infer the corresponding relation between the drugs and their places of origin (or growth location). Such analysis data of stable isotopes is significant for tracing the sources of drugs.

                Key words: forensic science; stable isotopes; drugs; traceability; synthetic pathways; place of origin

                引用本文:趙志東,孟嬌,鞏京慧,等. 穩定性同位素分析在毒品溯源中的應用研究進展[J]. 化學試劑,2022,44(9)1376-1384.

                 

                 

                多環芳烴類標準物質使用的穩定性評價

                 

                馬宇熙1,2,張瑩2,房苗2,阿力騰巴特2,孫向濤*2

                1. 新疆醫科大學 新疆特殊環境與健康研究重點實驗室,新疆 烏魯木齊  830054

                2. 烏魯木齊市疾病預防控制中心,新疆 烏魯木齊  830026

                 

                摘要:為了對以不同溶劑為介質的多環芳烴混合標準溶液儲存的穩定性進行了考察,選取200 mg·L-116種多環芳烴混合標準溶液,分別用乙腈和50%的乙腈配制成20 mg·L-1的中間液,在不同溫度(-18 ℃、4 ℃)下避光儲存、并于第7、15、30、60 d時用高效液相色譜對其特性量值進行測量。結果表明,標準溶液的特性量值在第一周就迅速衰減,7 ~ 30 d成直線下降趨勢,且4 ℃-18 ℃的衰減現象更明顯,30 ~ 60 d時呈現負增長現象,說明溶劑蒸發逃逸是引起溶質濃縮導致量值增大的重要原因。多環芳烴類的混合標準溶液經開封稀釋后不推薦重復使用,建議現用現配。

                關鍵詞:多環芳烴;標準物質;混合標準溶液;穩定性;評價;

                中圖分類號:O652.3    文獻標志碼:A      文章編號:0258-32832022

                 

                Stability Evaluation for the Application of Polycyclic Aromatic Hydrocarbon Standards MA Yu-xi1,2, Zhang Ying2, FANG Miao2, ALITENGBATE2, SUN Xiang-tao*2 (1. Xinjiang Medical University Key Laboratory of Special Environment and Health Research in Xinjiang, Urumqi 830054, China; 2. Urumqi Centre for Disease Control and Prevention, Urumqi 830026, China), Huaxue Shiji, 2022,

                Abstract: In order to investigate the storage stability of polycyclic aromatic hydrocarbons (PAHs) mixture standards with other different solvents, 16 kinds of PAHs (200 mg/L) mixture standards were selected as models to prepare intermediates (20 mg/L) by using acetonitrile and 50% acetonitrile, respectively. The obtained intermediates were stored at different temperatures (-18, 4℃) under dark condition, their characteristic values were subsequently monitored by high performance liquid chromatography on day 7, 15, 30 and 60. The results show that the characteristic values of standards decrease rapidly in the first week, and plummets from 7 to 30 days. Such attenuation phenomenon is more obvious at 4℃ than -18℃, and the negative growth phenomenon occurs from 30 to 60 days, suggesting the evaporation and escape of the solvent play important factor on inducing the concentration of the solute and thus increasing the characteristic values. Therefore, it will not be recommended to reuse the PAHs mixture standards once opened and diluted.

                Key words: polycyclic aromatic hydrocarbons (PAHs); reference materials;mixture standards; stability;evaluation;

                引用本文馬宇熙, 張瑩, 房苗, . 多環芳烴類標準物質使用的穩定性評價[J]. 化學試劑, 2022, 4491385-1392.

                 

                 

                抗癌藥艾樂替尼關鍵中間體的合成工藝改進

                田巖1,2,吳芳珍*1,黃一波1,張奉志3,張萬妹1,蘇怡1

                (1.常州工程職業技術學院 檢驗檢測認證學院,江蘇 常州  230031;2.東華大學 化學化工與生物工程學院,上海  201620;3.棗莊市潤安制藥新材料有限公司,山東 棗莊  277101)

                摘要:對艾樂替尼(Alectinib)關鍵中間體2-(4-乙基-3-碘苯基)-2-甲基丙酸的合成工藝進行了改進。以廉價易得的2-甲基-2-苯基丙酸為原料,通過縮合、傅克、還原、水解、碘代等反應得到的目標產物,HPLC測定目標化合物的純度為99.1%,整個合成路線中無需使用昂貴金屬催化劑,反應條件溫和,易于控制,并且可以以克級規模對中間體進行中試生產,總合成收率高達58%。改進后的工藝操作簡單、成本低廉、易于工業化放大,為艾樂替尼關鍵中間體的合成提供了一種新的、高效的制備方法。

                關鍵詞艾樂替尼;縮合;還原;碘代;合成工藝

                中圖分類號:O621.3    文獻標識碼:A       文章編號:0258-32832022--

                 

                Synthesis Improvement of Key Intermediates of Anticancer Drug Alectinib TIAN Yan1,2, WU Fang-zhen*1, HUANG Yi-bo1, ZHANG Feng-zhi3, ZHANG Wan-mei1, SU Yi1 (1. Inspection and Testing Certification Institute, Changzhou Vocational Institute of Engineering, Changzhou 213164, China; 2. College of Chemistry, Chemical Engineering and Biotechnology, Donghua University, Shanghai 201620, China;3. Zaozhuang Run'an Pharmaceutical New Material Co., Ltd., Zaozhuang, Shandong 277101), Huaxue Shiji, 2022, 44(9),

                Abstract: In this study, the synthesis of 2-(4-ethyl-3-iodophenyl)-2-methylpropanoic acid, a key intermediate of Alectinib, was improved. Using cheap and easily available 2-methyl-2-phenylpropionic acid as a raw material, the target product is obtained by condensation, Friedel-Crafts, reduction, hydrolysis, iodination and other reactions, and purity of compound is determined to be 99.1% by HPLC. This entire synthesis route does not require expensive metal catalysts, the reaction conditions are mild and easy to control, and the intermediate can be produced on a gram scale in a pilot, with a total synthesis yield of up to 58%. The improved process has the advantages of simple operation, low cost and easy industrial scale-up, and provides a new and efficient preparation method for the synthesis of key intermediates of Alectinib.

                Key wordsalectinib; condensation; reduction; iodine; synthesis

                引用本文:田巖,吳芳珍,黃一波,等. 抗癌藥艾樂替尼關鍵中間體的合成工藝改進[J]. 化學試劑,2022,44(9): 1393-1397。

                 

                 

                乙內酰脲衍生物RU58841的合成工藝研究

                王曉霞1,2,曹碧霞1,2,楊欣梓1,2,李澤坤3,劉榮*1,2

                (1. 甘肅省化工研究院有限責任公司,甘肅 蘭州  730020;2. 甘肅省精細化工重點實驗室,甘肅 蘭州  730020;3. 西北民族大學 化工學院,甘肅 蘭州  730030)

                摘要乙內酰脲是一種具有廣泛的生物和藥理活性,且具有4個功能點的五元雜環化合物。這種小而剛性的骨架可以有效地作用于各種藥理靶點,幾種臨床上重要的藥物如苯妥英(抗癲癇藥)、阿齊利特(抗心律失常藥)和尼魯米特(抗雄激素藥)等都是基于這種特征性的主要骨架。RU58841IUPAC 名稱:4-[3-4-羥基丁基)-4,4-二甲基-2,5-二氧咪唑啉-1-]-2-(三氟甲基)苯甲腈)是一種具有抗禿發活性的乙內酰脲衍生物,證據表明RU58841幾乎沒有毒性,有望成為一種新的外用非甾體抗雄激素。研究發現以4-氨基-2-(三氟甲基)芐腈為原料,通過三光氣制備異氰酸酯、[3+2]環加成、N -烷基化和脫保護共4步反應制備RU58841,總產率為40%。與傳統方法相比,該方法可以更方便、更安全地獲得RU58841。

                關鍵詞:三光氣;乙內酰脲;RU58841;[3+2]環加成;抗禿發劑

                中圖分類號:O62       文獻標識碼:A       文章編號:0258-32832022--

                 

                A New Method for Synthetic Methods of Hydantoin Derivative RU58841 WANG Xiao-xia1,2, CAO Bi-xia1,2, YANG Xin-zi1,2, LI Ze-kun3, LIU Rong *1,2 (1. Gansu Chemical Industry Research Institute Co. Ltd., Lanzhou 730020, China; 2. Key Laboratory of Fine Chemicals, Gansu Province. Lanzhou 730020, China; 3. Department of Chemistry, Norhwest Minzu University, Lanzhou 730030, China), Huaxue Shiji, 2022, 44(9),

                AbstractHydantoinis, a five-membered heterocyclic compound with four functional points, show various amazing biological and pharmacological activity. This small and rigid backbone could effectively act on various pharmacological targets. Several clinically important medicines such as phenytoin (antiepileptic), azimilide (antiarrhythmic) and nilutamide (antiandrogen) are based upon this characteristic staple scaffold. RU58841(IUPAC name: 4[3(4hydroxybutyl)4,4dimethyl2,5dioxoimidazolidin1yl]2(trifluoromethyl)benz onitrile) was found active against baldness with little evidence of toxicity, and it has promise as a new topically active non-steroidal antiandrogen. In this paper, we report a new alternative synthesis of RU58841. RU58841 was synthesized using 4-amino-2-(trifluoromethyl) benzonitrile as raw material in 4 steps including the preparation of isocyanate, [3+2] cycloaddition, N-alkylation and deprotection with over-all yield of 40%. Compare to traditional method, the method can be more convenient and safer to get RU58841.

                Key wordstriphosgene; hydantoin; RU58841; [3+2] cycloaddition; against baldness

                引用本文:王曉霞,曹碧霞,楊欣梓,等. 乙內酰脲衍生物RU58841的合成工藝研究[J]. 化學試劑,2022,449:1398-1402.

                 

                 

                2022化學試劑第9期PDF文檔.pdf

                 

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