《化学试剂》2017年第11期中英文摘要-东台市亚博化学试剂有限公司
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【亚博】硝酸铵产能已经过剩

作者:东台市亚博化学试剂有限公司    时间:2014-09-23    点击:1453

介孔TiO2中空微球的制备及其光催化功用研讨

石凯,李巧玲*

(中北大学 理学院,山西 太原 030051

摘要:选用双模板辅佐,经水热条件下制备出TiO2@C复合微球,高温煅烧除掉模板得到介孔TiO2中空微球。运用XRDSEMTEM和氮气吸脱-脱附仪对所制备样品的晶体结构、描摹及孔结构进行表征。所制备的介孔TiO2中空微球归于锐钛矿型,是由很多直径为15.31 nm的介孔初级微球堆积而成,全体微球直径约为360 nm,参加葡萄糖作为模板剂能使孔道结构变得有序。以罗丹明B为模仿污染物,讨论了介孔TiO2中空微球光催化降解罗丹明B的功用。成果标明,在20 W紫外光照耀下,50 mg介孔TiO2中空微球在30 min内可使初始浓度为10 mg/L的罗丹明B彻底降解,重复运用11次,在50 min时的降解率仍可达89.5%

要害词:二氧化钛;模板法;介孔;光催化功用;罗丹明B

中图分类号:O641.2 文献标识码:A 文章编号:0258-32832017

Preparation and Photocatalytic Properties of Mesoporous Hollow TiO2 Microspheres SHI Kai, LI Qiao-ling*(School of science, North University of China, Taiyuan 030051 )

Abstract:TiO2 mesoporous hollow microspheres (MHMs) were prepared by double-template method viacalcinatingpercussive TiO2@C spherical composites that were hydrothermally prepared. As-obtained products were characterized XRD, SEM, TEM, and nitrogen adsorption-desorption apparatus to reveal the crystal structure and morphology. Results showed that the TiO2 MHMs are in anatase phase, constructed by large amount of mesoporous primary microspheres whose diameter is 15.31 nm. The overall diameter of TiO2 MHMs is about 360 nm. Adding glucoses as template can result in ordered pore structure. Photocatalytic degradation of Rhodamine B was conveyed as the probe reaction to evaluate the photocatalytic activity of TiO2 MHMs. Results showed that Rhodamine B (10 mg/L) could be completely degraded in 30 min under ultraviolet light irradiation (20 W) using 50 mg mesoporous hollow TiO2 microspheres. As-made TiO2 MHMs can be recyclable, the degradation rate still reached 89.5% at the 11th use.

Key words:titania;template method;mesoporous; photocatalytic properties;Rhodamine B


Pd/CNTs金属纳米催化剂的制备及其催化对氯硝基苯加氢功用

张瀚1, 2王磊2胡广林1熊春荣1尹宏峰*2

1.海南大学 资料与化工学院,海南 海口 5702282.中国科学院 宁波资料技能与工程研讨所,浙江 宁波 315201

摘要:通过硝酸浸渍法对碳纳米管(CNTs)进行预处理改性,并选用乙二醇液相复原法制备Pd/CNTs纳米催化剂,通过XRD、TEM、BET、Raman spectra、ICP等手法对其进行了表征。成果标明,Pd/CNTs催化剂中Pd的负载量为0.9%,Pd纳米颗粒均匀地涣散在CNTs外表,粒径均匀巨细为5 nm。该催化剂用于对氯硝基苯的挑选加氢反响,在常压、60 ℃下反响2 h,该反响转化率为94.7%,挑选性为89.2%。

要害词:碳纳米管;钯;对氯硝基苯;挑选加氢;对氯苯胺

中图分类号O643.36 文献标识码:A 文章编号:0258-3283(2017)

Preparation of Pt /CNTs Nano-catalyst and Performance in Hydrogenation of p- Chloronitrobenzene ZHANG Han1,2 , WANG Lei2, HU Guang-lin1, XIONG Chun-rong1, YIN Hong-feng*2(1.College of Materials and Chemical Engineering, Hainan University, Haikou 570228, China; 2. Ningbo Institute of Materials Technology and Engineering, Chinese Academy of Sciences, Ningbo 315201, China)

Abstract:Pd/CNTs nanocatalyst was prepared by pretreatment of carbon nanotubes (CNTs) followed with liquid phase reduction method. The catalyst was characterized by XRD, TEM, BET, Raman spectra and ICP. The results showed that the loading of palladium on Pd/CNTs catalyst was 0.9%, palladium nanoparticles highly dispersed on the surface of CNTs with average diameter of 5 nm. The catalyst was used for selective hydrogenation of chloronitrobenzene and the hydrogenation conversion was 94.7% and the selectivity was 89.2%.

Key wordsnanotubes; palladium; chloronitrobenzene; selective hydrogenation; chloroaniline

2-芳醛腙噻唑类化合物的组成及其抗肿瘤活性

李韦韦,姚敏娜,卜伟,王婧雯,文爱东*

(第四军医大学榜首隶属医院 药剂科,陕西 西安 710032)

摘要:噻唑环和腙键结构均具有必定的生物活性,选用活性结构拼接法,将噻唑环与腙键相结合,规划并组成了16个2-芳醛腙噻唑类化合物,并选用MTT法对方针化合物进行体外抗肿瘤活性挑选。测验成果标明,该类新化合物对乳腺癌细胞细胞系(MDA-MB-231、MDA-MB-468、MCF-7)具有必定的抗增殖活性。其间,N-(2-吡啶)甲醛-2-(4-苯基)噻唑腙的抗增殖活性最好,其IC50值别离为(0.21± 0.11)、(0.18 ± 0.10)、(0.17 ± 0.08)μmol/L;而该化合物对其他肿瘤细胞亦具有必定的抗增殖活性,且相对乳腺癌细胞株的生物活性均在10倍及以上,阐明其对乳腺癌细胞具有较好的生物活性和挑选性,且毒副效果小,值得作为抗乳腺癌先导化合物进行进一步研讨。

要害词噻唑环;腙键;乳腺癌细胞;抗增殖活性;挑选性

中图分类号R914.5 文献标识码:A 文章编号:0258-32832017

Synthesis and Antitumor Activity of 2-Thiazolylhydrazyne Scaffold Derivatives LI Wei-wei, YAO Min-na, BU Wei, WANG Jing-wen, WEN Ai-dong* (Department of Pharmacy, Xijing Hospital, Fourth Military Medical University, Xi’an 710032, China)

Abstract:Thiazole ring and hydrazone structure have certain biological activity. In this work, we applied the active structure-linking method, which is combining thiazole and hydrazone, and have designed and synthesized a series of novel 2-thiazolylhydrazyne scaffold derivatives.The structures were confirmed by 1HNMR and elemental analysis. These compounds were evaluated for anti-breast cancer activity on MDA-MB-231, MDA-MB-468, MCF-7 cells by MTT method in vitro. The test results show that this kind of new compounds has antiproliferative activity. And N-(4-phenyl-thiazole- 2-yl)-2-pyridine hydrazone exhibited better antiproliferative activity against MDA-MB-231, MDA-MB-468, MCF-7breast cells with the IC50 value of 0.21±0.11、0.18±0.10、0.17±0.08 μmol/L, respectively.This compound also has certain antiproliferative activity against the other tumor cells (PANC-1, Hela, MKN45, SKOV3, Karpas299, Ramos). And the relate selectivity of compound against MDA-MB-231 cell are more than 10 times. The results show that it has good biological activity and selectivity against breast cancer cells with low side effects. So above compound is worth as lead compound of breast cancer for further research.

Key words:thiazole; hydrazone; breast cancer cells; antiproliferative activity; selectivity


2-芳醛腙噻唑类化合物的组成及其抗肿瘤活性

李韦韦,姚敏娜,卜伟,王婧雯,文爱东*

(第四军医大学榜首隶属医院 药剂科,陕西 西安 710032)

摘要:噻唑环和腙键结构均具有必定的生物活性,选用活性结构拼接法,将噻唑环与腙键相结合,规划并组成了16个2-芳醛腙噻唑类化合物,并选用MTT法对方针化合物进行体外抗肿瘤活性挑选。测验成果标明,该类新化合物对乳腺癌细胞细胞系(MDA-MB-231、MDA-MB-468、MCF-7)具有必定的抗增殖活性。其间,N-(2-吡啶)甲醛-2-(4-苯基)噻唑腙的抗增殖活性最好,其IC50值别离为(0.21± 0.11)、(0.18 ± 0.10)、(0.17 ± 0.08)μmol/L;而该化合物对其他肿瘤细胞亦具有必定的抗增殖活性,且相对乳腺癌细胞株的生物活性均在10倍及以上,阐明其对乳腺癌细胞具有较好的生物活性和挑选性,且毒副效果小,值得作为抗乳腺癌先导化合物进行进一步研讨。

要害词噻唑环;腙键;乳腺癌细胞;抗增殖活性;挑选性

中图分类号:R914.5 文献标识码:A 文章编号:0258-32832017

Synthesis and Antitumor Activity of 2-Thiazolylhydrazyne Scaffold Derivatives LI Wei-wei, YAO Min-na, BU Wei, WANG Jing-wen, WEN Ai-dong* (Department of Pharmacy, Xijing Hospital, Fourth Military Medical University, Xi’an 710032, China)

Abstract:Thiazole ring and hydrazone structure have certain biological activity. In this work, we applied the active structure-linking method, which is combining thiazole and hydrazone, and have designed and synthesized a series of novel 2-thiazolylhydrazyne scaffold derivatives.The structures were confirmed by 1HNMR and elemental analysis. These compounds were evaluated for anti-breast cancer activity on MDA-MB-231, MDA-MB-468, MCF-7 cells by MTT method in vitro. The test results show that this kind of new compounds has antiproliferative activity. And N-(4-phenyl-thiazole- 2-yl)-2-pyridine hydrazone exhibited better antiproliferative activity against MDA-MB-231, MDA-MB-468, MCF-7breast cells with the IC50 value of 0.21±0.11、0.18±0.10、0.17±0.08 μmol/L, respectively.This compound also has certain antiproliferative activity against the other tumor cells (PANC-1, Hela, MKN45, SKOV3, Karpas299, Ramos). And the relate selectivity of compound against MDA-MB-231 cell are more than 10 times. The results show that it has good biological activity and selectivity against breast cancer cells with low side effects. So above compound is worth as lead compound of breast cancer for further research.

Key words:thiazole; hydrazone; breast cancer cells; antiproliferative activity; selectivity

新式复合资料MnFe2O4@SiO2-NH2的制备

及其固定青霉素G酰化酶

杜传虎,薛屏*,谷耀华,胡春苗

(宁夏大学动力化工要点试验室,宁夏银川 750021

摘要:通过溶剂热法制备出高磁性的聚合物微球MnFe2O4,经正硅酸乙酯(TEOS)和3-氨基丙基三乙氧基硅烷(APTS)对微球外表进行改性润饰,制备出新式复合资料MnFe2O4@SiO2-NH2,并将其用于固定化青霉素G酰化酶。在Si/Fe比为7 mmol/g、n(TEOS): n(APTS) = 1:1时,固定化酶PGA/MnFe2O4@SiO2-NH2在37℃下水解青霉素G钾组成6-氨基青霉烷酸,表观酶活为1660 IU/g、载酶量为107.1 mg/g、比活性为15.5 IU/mg、活性回收率为46.9%。通过6次重复运用,保存初始酶活的81.3%,在运用中固定化酶在磁场的效果下能够快速沉降与产品别离。

要害词:磁性复合资料;固定化青霉素G酰化酶;催化活性

中图分类号:O643 文献标识码:A 文章编号:0258-32832017

Preparation of New Composite MnFe2O4@SiO2-NH2 and Immobilization for Penicillin G AcylaseDUChuan-hu,XUE Ping*, GU Yao-hua, HU Chun-miao(Key Laboratory of Energy Resources &Chemical Engineering , Ningxia University , Yinchuan 750021, China)

Abstract: High magnetic polymer microspheres MnFe2O4 were prepared by solvothermal method.Themagnetic composite materials MnFe2O4@SiO2-NH2were prepared by using tetraethoxysilane (TEOS) and 3-aminopropyl triethoxysilane (APTS) to decorating the surface of the microspheres MnFe2O4, and were used as the support for immobilization of penicillin G acylase (PGA).When the Si/Fe was 7 mmol/g and n(TEOS) :n(APTS ) = 1:1,the apparent activity of PGA/MnFe2O4@SiO2-NH2for hydrolyzing penicillin G potassium into6-aminopenicillanic acid at 37℃was 1660 IU/g, the enzyme load was about 107.1 mg/g, the specific activity was 15.5 IU/mg, and the activity recovery was about 46.9% and retained the initial activity of 81.3% after 6 recycles.The PGA/MnFe2O4@SiO2-NH2 can settle quickly in the magnetic field and be separated easily from the product in applications.

Key words:magnetic composite materials; immobilized penicillin G acylase; catalytic activity


去甲去氢斑蝥素酰亚胺衍生物的组成及抑菌活性

曾造*,李金海,舒群威,吕敬松

(贵州工程使用技能学院 化学工程学院 贵州省使用化学特征要点试验室,贵州 毕节 551700

摘要:以顺丁烯二酸酐和呋喃为开始质料,经Diels-Alder、替代和缩合反响,组成了7个去甲去氢斑蝥素酰亚胺衍生物,其结构经NMR和元素剖析证明。通过滤纸片法,别离测定组成物对大肠杆菌、金黄色葡萄球菌的抑菌活性。成果标明,中间体N-氨基去甲去氢斑蝥素酰亚胺和部分产品对两种细菌都有较好的抑菌活性。其间,N-(氨基缩对甲氧基苯甲醛)-去甲去氢斑蝥素酰亚胺对大肠杆菌的抑菌活性最强,抑菌圈直径为28 mm。

要害词:去甲去氢斑蝥素;酰亚胺衍生物;组成;抑菌活性

中图分类号: O625.6 文献标识码A 文章编号:

Synthesis and Bacteriostatic Activity of Dehydronorcantharidin Imide Derivatives ZENG Zao *, LI Jin-hai, SHU Qun-wei, LV Jing-song (Guizhou Key Laboratory of Applied Chemistry, School of Chemical Engineering, Guizhou University of Engineering Science, Bijie 551700, China)

Abstract: In this work, seven dehydronorcantharidin imide derivatives were synthesized through Diels-Alder,substitution and condensation from furan and maleic anhydride.The structures of synthetic compounds were confirmed by NMR and elemental analysis. The bacteriostatic activity of synthetic compounds against Escherichia coli and Staphylococcus aureus were tested by the method of filter-paper. The result shown that the N-amino dehydronorcantharidin and some compounds against twobacteria had obvious antibacterial activity. Especially, N-amino- 4-methoxybenzaldehyde dehydronorcantharidin against Escherichia coli was the best,and the inhibition zone diameter was 28 mm.

Key words: dehydronorcantharidin; imide derivatives; synthesis; bacteriostatic activity


反相微乳法制备DMCC用于催化二氧化碳与环氧丙烷共聚

周钰1, 2,唐喆1,许琦*1

(1. 盐城工学院化学化工学院,江苏盐城2240512.常州大学石油化工学院,江苏常州 213164)

摘要:通过反相微乳法和共沉淀法组成了钴锌双金属氰化物催化剂。研讨了制备办法及共聚反响条件对其催化功用及聚碳酸酯组成的影响。成果标明,反相微乳法制备的DMCC-1具有较低的结晶度且能够络合更多的有机配体,且在80℃、4MPa的条件下,选用一步加料法催化CO2与环氧丙烷共聚所制备的聚碳酸酯中碳酸酯单元量达43.5%,数均分子量达36400,且聚合物涣散指数仅为2.07。共聚成果标明一步加料法有利于进步聚合物的数均分子量,而逐渐加料法有利于下降聚合物的相对分子量散布。

要害词:双金属氰化物催化剂;反相微乳法;二氧化碳;环氧丙烷;聚碳酸酯

中图分类号:O643.32文献标识码:A 文章编号:0258-32832017

DMCC Prepared via Reverse MicroemulsionMethod and Catalytzed Copolymerization of Carbon Dioxide withPropylene Oxide ZHOU Yu1,2,TANG Zhe1, XU Qi*1(1. School of Chemistry and Chemical Engineering, Yancheng Institute of Technology, Yancheng 224051, China;2. College of Chemistry and Chemical Engineering, Changzhou University, Changzhou 213164, China)

Abstract:Cobalt zinc double metal cyanide catalysts were prepared by reverse micro emulsion method and coprecipitation method. The effect of preparation and reaction condition on catalytic performance and the polycarbonate composition were investigated. The results revealed that DMCC-1 prepared by reverse microemulsion method had lower crystallinity and complexed more organic ligand. The polycarbonate synthesized from CO2 and propylene oxide in the presence of DMCC-1 under the conditions of 80 °C,4 MPaandone-step feed modepossessed the molar fraction of carbonate linkages in the produced polymer was43.5%,number average molecular mass up to 36400 and polydispersity index was 2.07.At the same time, it was found that theone-step feed mode could improve the number average molecular of the polycarbonate, but interval feed mode could reduce thepolydispersity index of the polycarbonate.

Keywords: double metal cyanide catalyst; reverse microemulsionmethod; carbon dioxide; propylene oxide; polycarbonate

6-(呋喃-2-亚甲氨基)-2-甲基-1H-吲哚-3-羧酸乙酯的组成、表征与生物活性研讨

画莉1,万茂生*1,童张法2,陈丹1,李传宗1,苏月清1

(1. 贺州学院 资料与环境工程学院,广西 贺州 542899

(2. 广西大学 化学化工学院,广西 南宁 530004

摘要:以2, 4-二硝基氯苯为质料,通过3步反响得到标题化合物。当温度为78 ℃,反响时刻为8.5 h,方针化合物的收率可达65%。通过IR、1HNMR、13CNMR和MS光谱技能对其结构进行表征。运用SRB法点评了方针化合物对人体肺癌细胞成长按捺活性。开始的生物试验标明,该化合物对癌细胞H1792,A549,H157和Calu-1具有成长按捺效果,且具有浓度依赖性。细胞周期剖析发现其能诱导Calu-1细胞凋亡。

要害词:6-(呋喃-2-亚甲氨基)-2-甲基-1H-吲哚-3-羧酸乙酯;组成;表征;生物活性

中图分类号: O626.1 文献标识码: A 文章编号:0258-32832017

Synthesis, Characterization and Biological Activity of Ethyl 6-(Furan-2-ylmethyleneamino)-2-Methyl-1H-Indole-3-Carboxylate HUA Li1, WAN Mao-sheng*1, TONG Zhang-fa2, CHEN Dan1,LI Chuan-zong1, SU Yue-qing1(1.College of Material and Environmental Engineering, Hezhou University, Hezhou 542899, China; 2. School of Chemistry& Chemical Engineering, Guangxi University, Nanning 530004, China), Huaxue Shiji, 2017, 39(10)

Abstract:Ethyl 6-(furan-2-ylmethyleneamino)-2-methyl-1H-indole-3-carboxylate was synthesized via three-step reaction using 2, 4-dinitrochlorobenzene as the material. When the reaction temperature was 78℃ and reaction time was 8.5 h, the yield of target compound by the column chromatography reached 65%. The structure of compound was confirmed by IR, 1HNMR, 13CNMR and MS. Growth inhibitory activity of 6-(furan-2-ylmethyleneamino)-2-methyl-1H-indole-3-carboxylate on human lung cancer cells was evaluated by the method of SRB. The preliminary biological experiments showed that compound possessed growth inhibition activity to cancer cells H1792, A549, H157 and Calu-1 in a dosage dependent manner. It was found that compound induced apoptosis of Calu-1 cells by cell cycle analysis.

Key wordsEthyl 6-(furan-2-ylmethyleneamino)-2-methyl-1H-indole-3-carboxylate; synthesis; characterization; biological activity

化学计量银促进的偶联反响研讨开展

季玉雯,秦晓露,殷晓婷,胡静伟,王晨,程凯*

(绍兴文理学院 化学化工学院,浙江 绍兴 312000)

摘要:过渡金属银因为其催化反响契合绿色化学的准则,在有机组成中的使用成为近年来研讨的热门。但实际上化学计量的银往往被作为助剂以进步金属离子的反响活性,而银化合物自身作为催化剂的使用却非常有限。针对此类问题,近年来的作业会集在运用银合作物的σ-和π-路易斯酸性性质研讨银催化的反响。总述了银促进的偶联反响在C-P(N、S)键的构成和三氟甲基化反响研讨中的使用和开展。

要害词银促进;偶联反响;C-P(N、S)键的构筑;三氟甲基化反响

中图分类号:O621. 3 文献标识码:A 文章编号:0258-3283(2017)

Research Progress in Equivalent Ag-Mediated Coupling Reactions JI Yu-wen, QIN Xiao-lu, YIN Xiao-ting, HU Jing-wei, WANG Chen, CHENG Kai * (College of Chemistry and Chemical Engineering,Shaoxing University,Shaoxing 312000,China) Huaxue Shiji,2017,39

AbstractThe application of transition metal silver in organic synthesis has been a hot topic in recent years because of its catalytic reaction to the principle of green chemistry. But in fact, the silver of stoichiometry is often used as an auxiliary agent to improve the reaction activity of metal ions while the use of silver compounds as catalysts is very limited. In response to such problems, the work in recent years has focused on the study of silver catalytic reactions using the sigma - and pi-lewis acid properties of the silver complex. Equivalent Ag-mediated coupling reactions has been widely studied in organic synthesis. The research progress on Ag-mediated cross-coupling is reviewed, focusing on applications and progress of the construction of C-P(N, S) bonds and trifluoromethylation.

Key wordsAg-mediated; coupling reaction; construction of C-P(N, S) bonds; trifluoromethylation

分子印迹固相萃取技能在食物安全检测中的使用开展

田春霞

(北京有色金属研讨总院,北京100088

摘要:分子印迹固相萃取技能(MISPE)是一种高效的样品前处理技能,能从杂乱的样品中挑选性别离方针物及其结构类似物。分子印迹技能( MIT) 在食物中农药和兽药残留检测中的使用快速开展。总述了近两年国表里分子印迹固相萃取技能在食物安全检测中农药、兽药残留检测的使用及开展,评论了当时分子印迹固相萃取技能在食物安全检测使用中存在的问题,并对其开展趋势进行了展望。

要害词:分子印迹固相萃取技能(MISPE);食物安全;农药和兽药残留;使用开展

中图分类号O658 文献标识码:A 文章编号:0258-32832017

Application Developmentof Molecularly Imprinted Solid-phase Extraction Technologyon Detection in Food Safety TIAN Chun-xia (Beijing General Research Institute for Nonferrous Metals, Beijing 100088)

Abstract: Molecularly imprinted solid-phase extraction technology (MISPE) is a sample pretreatment technology with high performance, which can separate target molecules and structurally similar molecules from complex samples selectively. Applications of molecular imprinted technology ( MIT) on detection of pesticide residues and veterinary drugs residues in food have been developed rapidly. This paper reviews application development of molecularly imprinted solid-phase extraction technology on detection in food safety in recent two years. Besides, the current problems and the future development of the technology are discussed.

Key words: molecularly imprinted solid-phase extraction(MISPE); food safety; pesticides residues and veterinary drugs residues; application development

金属合作物抗癌活性的研讨开展

吴月红

(吉林工程职业学院 粮食与食物工程学院,吉林 四平 136000

摘要:自从发现顺铂具有抗癌活性以来,金属合作物作为新一类抗癌药物引起了人们的广泛重视。总述了近年来铂类合作物、钌类合作物和席夫碱合作物在抗癌药物中的研讨开展,要点论述了铂类合作物抗癌活性的研讨现状及效果原理,并对金属合作物抗癌活性的研讨开展进行总结,为金属合作物抗癌药物研讨供给参阅和根据。

要害词:金属合作物;抗癌活性;铂类合作物;钌类合作物

中图分类号:O641.4 文献标识码:A 文章编号:0258-32832017

Progress in Anticancer Activity of Metal Complexes WU Yue-hong ( , Jilin Engineering Vocational College, Siping 136000, China), Huaxue Shiji, 2017, 39(10)

Abstract: Since the discovery of the anticancer activity of cisplatin, as a new class of anticancer drugs, metal complexes have attracted extensive attention. Recent advances in the researches on platinum complexes, ruthenium complexes and Schiff bases in anticancer drugs are reviewed. The research status and principle of the anticancer activity of platinum complexes are emphasized. And the research progress of the anticancer activity of metal complexes is summarized. It provides reference and basis for the new research field of anticancer drugs of metal complexes.

Key words: metal complexes; anticancer activity; platinum complexes; ruthenium complexes


高效液相色谱-串联质谱法测定粮谷中十二环吗啉和十三吗啉残留量

曹海微1,田芳洁2,康明芹1*,李荣荣1,杨璐1,顾婷婷1

1. 吉林出入境检验检疫局,吉林 长春 130062

2. 长春市食物药品监督管理局南关监督管理所,吉林 长春 130062

摘要:建立了高效液相色谱-串联质谱法(HPLC-MS/MS)测定粮谷中十二环吗啉和十三吗啉残留量的剖析办法。样品经1%甲酸-乙腈超声提取,石墨化炭黑/氨基复合固相萃取柱净化,HPLC-MS/MS多反响监测形式测定,外标法定量。成果标明,十二环吗啉和十三吗啉在2.0 ~ 200.0 µg/L范围内线性关系杰出,相关系数均大于0.999。本办法十二环吗啉和十三吗啉的定量限别离为2.0 μg/kg和5.0 μg/kg,样品基质中两种方针物在3个增加水平的均匀回收率为78.0 % ~ 96.0 %,相对规范偏差(RSD)为3.0 % ~ 8.2 %。该办法简略、活络、准确、牢靠,可用于粮谷中十二环吗啉和十三吗啉残留剖析。

要害词:高效液相色谱-串联质谱;粮谷;十二环吗啉;十三吗啉

中图分类号:O657.63 文献标识码:A 文章编号:0258-32832017

Determination of Dodemorph and Tridemorph in Grain using High Performance Liquid Chromatography-tandem Mass Spectrometry CAO Hai-wei, TIAN Fang-jie, KANG Ming-qin*, LI Rong-rong, YANG lu, GU Ting-ting1. Quarantine Technology Center of Jilin Entry-Exit Inspection and Quarantine Bureau, Changchun 130062; 2. Nanguan Supervision Institute of Changchun food and Drug Administration Inspection, Changchun 130062

Abstract: High performance liquid chromatography-trandem mass spectrometry(HPLC-MS/MS) was applied to determine the dodemorph and tridemorph residues in grain.The analytes in samples were extracted using 0.1 % formic acid - acetonitrile mixture as the extraction solvent and were further purified with the ENVI-Carb/LC cartridge. The purified liquid was detected using HPLC-MS/MS and quantified usingexternalstandard method. The results showed that the good linear range for dodemorph and tridemorph were 2.0 ~ 200. 0 μg/L, and the correlation coefficients were higher than 0. 999. The limit of quantification for the dodemorph and tridemorph was 2.0 μg/kg and 5.0 μg/kg respectively. The recoveries of the analytes at three spiked levels ranged between 78.0 % and 96.0 % with the relative standard deviations of 3.0 % ~ 8.2 %. The present method is simple, sensitive, reliable and accurate which can be suitible for dodemorph and tridemorphanalysis of grain.

Key words: HPLC-MS/MS; grain; dodemorph; tridemorph

异烟酸-吡唑啉酮光度法测定硫酸铵中氰化物

方诚,凌芳*,郑琦,陈浩云

(国药集团化学试剂有限公司,上海200002

摘要:本文通过从样品成分特色和测验原理下手,对异烟酸-吡唑啉酮光度法测定硫酸铵中氰化物的影响要素作了开始剖析和评论。其间对试验过程中样品取样量、显色系统pH、显色温度、显色反响时刻及氧化剂的挑选进行了优化。测验成果显现,本办法的最佳取样量为0.1g,最佳显色温度为35℃,最佳反响时刻为40 min,线性回归方程Y=0.0025+2.1168 X,办法检出限为0.0014 μg/mL。该研讨为往后硫酸铵中氰化物的测定供给了必定的技能支撑。

要害词:硫酸铵;异烟酸-吡唑啉酮光度法;氰化物

中图分类号:O623.76 文献标识码:A 文章编号:

IsonicotinicAcid – pyrazoloneSpectrophotometric Determination of Cyanide in Ammonium Sulfate FANG Cheng, LING Fang*, ZHENG QiCHEN Hao-yunSinopharm Chemical Reagent Co., LTD , Shanghai200002

AbstractIn this paper, the factors affecting the determination of cyanide in ammonium sulfate are analyzed and discussed starting with the composition, characteristics and testing principle of the sample. The sample size, color rendering system, pH, color rendering temperature, color reaction time and oxidant selection were optimized.The results show the optimum sampling weights was 0.1g,the optimum temperature was 35℃ and the optimum time was 40 min. The linear equation is Y=0.0025+2.1168X.The detection limit was 0.0014μg/mL.The cyanide in ammonium sulfate was determined by isonicotinicacid-pyrazolonespectrophotometry.

Keywords:ammonium sulfate; is

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