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Sephadex G-10凝胶色谱系统测定头孢西丁钠中高分子聚合物

【英文篇名】Determination of HMW Impurities of Cefoxitin Sodium by Sephadex G-10 Chromatographic System
【作者中文名】刘云; 高燕霞; 姜建国;
【作者英文名】Liu Yun; Gao Yan-xia; Jiang Jian-guo(Hebei Institute for Drug Control; Shijiazhuang 050011);
【作者单位】河北省药品检验所;
【文献出处】中国药品标准, Drug Standards of China, 编辑部邮箱 2009年 02期 
期刊荣誉:ASPT来源刊  CJFD收录刊
【关键词】高分子聚合物; 头孢西丁; Sephadex G-10凝胶色谱系统;
【英文关键词】HMW Impurities; Cefoxitin Sodium; Sephadex G-10 Chromatographic System;
【摘要】目的:建立测定头孢西丁钠中高分子聚合物的含量。方法采用Sephadex G-10凝胶色谱系统。色谱柱:葡聚糖凝胶G-10色谱柱;流动相A:pH7.0的0.1mol.L-1磷酸盐缓冲液[0.1mol.L-1磷酸氢二钠溶液-0.1mol.L-1磷酸二氢钠溶液(61∶39)],流动相B:超纯水;流速:1.0mL·min-1,检测波长:254nm。结果:头孢西丁钠高分子聚合物在5~70g.L-1的范围内线性关系良好,r=0.9943。结论:本方法专属性强,准确度高、重现性好,可作为头孢西丁钠中高分子聚合物含量的测定方法。
【英文摘要】Objective:To develop a method for determination of HMW Impurities of Cefoxitin Sodium.Methods:Sephadex G-10 column;Mobile phase A:0.1 mol·L-1 phosphate buffer(pH 7.0);Mobile phase B:water;Flow rate:1.0 mL·min-1;wavelength:254 nm.Results:The linear range for HMW Impurities of Cefoxitin Sodium was 5~70 g·L-1(r=0.994 3).Conclusion:The method was convenient,specific,accurate and can be used for determination of HMW Impurities of Cefoxitin Sodium.
【DOI】CNKI:SUN:YPBZ.0.2009-02-019
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凝胶渗透色谱-气相-质谱测定鲸皮脂中的多氯联苯

【英文篇名】Determination of residual polychlorinated biphenyls (PCBs) in blubber of whale by gel permeation chromatography and gas chromatography/mass spectrometry
【作者中文名】黄健生; 卢伟华; 邹潍力; 王耀;
【作者英文名】HUANG Jiansheng; LU Weihua; ZOU Weili; WANG Yao(Dongguan Marine and Fishery Environment Monitoring Station; Dongguan 523888; China);
【作者单位】东莞市海洋与渔业环境监测站;
【文献出处】南方水产, South China Fisheries Science, 编辑部邮箱 2009年 04期 
期刊荣誉:ASPT来源刊  CJFD收录刊
【关键词】多氯联苯; 鲸; 凝胶渗透色谱; 气质联仪;
【英文关键词】polychlorinated biphenyls; whale; gel permeation chromatography; gas chromatography/mass spectrometry;
【摘要】建立了一种测定鲸皮脂中多氯联苯(PCBs)前处理的改良方法,即将皮脂样品分别经超声波萃取、GPC净化和浓缩等处理后,用GC-MS测定。结果显示,该方法加标回收率为73%~118%,精密度为4.1%~9.7%,检出限在0.19~1.07ng.g-1之间。该方法操作简单,净化效果好、准确性高、重复性强,适合鲸皮脂中PCBs含量的分析测定。
【英文摘要】An ameliorated pretreatment method for determination of polychlorinated biphenyls(PCBs)in blubber of whale has been established. The samples were extracted with ethyl acetate-cyclohexane by ultrasonically assisted procedure. The extract was purified and condensed with GPC and PCBs were determined by GC-MS.The results showed that the recoveries of spiked matrix were between 73% and 118%,the coefficient of variation was 4.1%~9.7%. The detection limits of the method were 0.19~1.07 ng·g-1. This method,with easy...
【基金】农业部渔业生态环境重点开放实验室开放基金项目(2007-13);; 科技部科研院所社会公益研究专项(2005DIB3J021)
【DOI】CNKI:SUN:NFSC.0.2009-04-003
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凝胶色谱实验条件对聚醚多元醇相对分子质量测定的影响

【英文篇名】The Effect of GPC Experimental Conditions on the Average Molecular Weight of Polyether Polyols Determination
【作者中文名】程广斌; 卢波;
【作者英文名】Cheng Guangbin Lu Bo(School of Chemical Engineering; Nanjing University of Science and Technology; Nanjing 210094; China);
【作者单位】南京理工大学化工学院;
【文献出处】聚氨酯工业, Polyurethane Industry, 编辑部邮箱 2009年 03期 
期刊荣誉:中文核心期刊要目总览  ASPT来源刊  CJFD收录刊
【关键词】凝胶渗透色谱; 聚醚多元醇; 实验条件; 相对分子质量;
【英文关键词】gel permeation chromatography; polyether polyol; experimental condition; average molecular weight;
【摘要】凝胶渗透色谱(GPC)测定聚醚多元醇的相对分子质量及其分布。以四氢呋喃作为溶剂和流动相,探讨了样品浓度、色谱柱温度以及流动相流速等条件对实验结果的影响。结果表明,样品浓度控制在1.0~3.0 mg/mL,且保证待测样品浓度与标准样品浓度一致时,实验结果误差较小;实验温度在30~50℃范围内对结果影响不大;流速低于1 mL/min时结果出现较小偏差;重复性测定平均相对分子质量的相对标准偏差仅有1%。
【英文摘要】Gel Permeation Chromatography(GPC) was used to determine the distribution and average molecular weight of polyether polyols.Tetrahydrofuran(THF) was used as solvent and the different experimental conditions were discussed.The results showed that the relative error of the results was small when the concentration of the sample solutions in THF were between 1.0~3.0 mg/mL and was exactly the same as the concentration of standard samples.The results which were obtained at different column temperatures between 30...
【DOI】CNKI:SUN:JAZG.0.2009-03-014
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加速溶剂萃取凝胶色谱净化气相色谱-质谱联用测定土壤中多环芳烃

【英文篇名】Determination of Polycyclic Aromatic Hydrocarbons in Soil by GC/MS with Accelerated Solvent Extraction and Gel Permeation Chromatographic Cleanup
【作者中文名】王志; 李洁; 李振国;
【作者英文名】WANG Zhi LI Jie LI Zhen-Guo(Dalian Environmental Center; Dalian; Liaoning 116023; P.R.China);
【作者单位】大连市环境监测中心;
【文献出处】光谱实验室, Chinese Journal of Spectroscopy Laboratory, 编辑部邮箱 2009年 04期 
期刊荣誉:中文核心期刊要目总览  ASPT来源刊  CJFD收录刊
【关键词】多环芳烃; 加速溶剂萃取; 凝胶色谱; 气相色谱-质谱法;
【英文关键词】PAHs; ASE; GPC; GC/MS;
【摘要】土壤样品经过加速溶剂萃取仪与凝胶色谱净化浓缩提纯处理后,用气相色谱-质谱联用仪测定土壤中多环芳烃。
【英文摘要】The Polycyclic Aromatic Hydrocarbons(PAHs)in soil were pretreated by Accelerated Solvent Extraction(ASE) and gel permeation chromatograph(GPC),and determined by GC/MS.
【DOI】CNKI:SUN:GPSS.0.2009-04-020
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凝胶渗透色谱及固相萃取技术测定蔬菜中20种农药的残留

【英文篇名】Determination of Twenty Pesticide Residues in Vegetable by Gel Permeation Chromatography and Solid Phase Extraction
【作者中文名】沈涛; 沈水荣; 姚艳玲;
【作者英文名】SHEN Tao; SHEN Shui-rong; YAO Yan-ling (Jiaxing Agriculture Products Supervision & Teting Agency; Zhejiang Province; Jiaxing 314033; China);
【作者单位】浙江省嘉兴市农产品监测中心;
【文献出处】上海交通大学学报(农业科学版), Journal of Shanghai Jiaotong University(Agricultural Science), 编辑部邮箱 2009年 01期 
期刊荣誉:ASPT来源刊  CJFD收录刊
【关键词】凝胶渗透色谱; 固相萃取; 农药残留; 蔬菜;
【英文关键词】gel permeation chromatography; solid phase extraction; pesticide residue; vegetable;
【摘要】采用凝胶渗透色谱(GPC)净化结合固相萃取技术,建立了蔬菜中α-六六六、β-六六六、γ-六六六、δ-六六六、百菌清、艾氏剂、三唑酮、噻嗪酮、p,p'-DDE、狄氏剂、o,p'-DDT、p,p'-DDD、p,p'-DDT、联苯菊酯、甲氰菊酯、氯菊酯、氯氟氰菊酯、氯氰菊酯、氰戊菊酯、溴氰菊酯等20种有机氯和拟除虫菊酯类农药残留的气相色谱(GC-ECD)检测方法。结果表明,供试的20种农药分离状况良好,黄瓜中添加0.01~1.0 mg·kg~(-1)水平的农药,回收率为69.2%~116.3%,相对标准偏差为1.4%~8.9%,最低检出限为0.06~13.0μg·kg~(-1)。结果证明,该方法回收率、精密度、最低检出限均能满足农药残留检测要求。
【英文摘要】A vegetable testing method using GC-ECD with pretreatments of gel permeation chromatography and solid phase extraction to determine 20 types of organochlorine pesticides and pyrethroid pesticides was studied,involvedα-666,β-666,γ-666,δ-666, chlorothalonil,aldrin,triadimefon,buprofezin,p,p -DDE,dieldrin,o,p -DDT,p,p -DDD,p,p -DDT,bifenthrin,fenpropathrin,permethrin, cyhalothrin,cypermethrin,fenvalerate,deltaraethrin,etc.The results indicated that the 20 pesticides had well separation.We added pesticides with...
【基金】2007年嘉定市科技计划项目(No.2007AY2003)
【DOI】CNKI:SUN:SHNX.0.2009-01-016
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凝胶渗透色谱-固相萃取净化测定茶叶中16种菊酯残留量

【作者中文名】丁慧瑛; 谢文; 蒋晓英; 李铂; 黄雷芳;
【作者单位】浙江出入境检验检疫局;
【文献出处】分析试验室, Chinese Journal of Analysis Laboratory, 编辑部邮箱 2009年 S1期 
期刊荣誉:中文核心期刊要目总览  ASPT来源刊  CJFD收录刊
【关键词】凝胶渗透色谱; 气相色谱-质谱; 负化学源; 茶叶; 菊酯; 残留;
【摘要】建立了以凝胶渗透色谱(GPC)和固相萃取(SPE)净化,气相色谱-质谱(GC-MS)负化学源(NCI)技术测定茶叶中七氟菊酯、四氟菊酯、丙烯菊酯、联苯菊酯、胺菊酯、甲氰菊酯、氯氟氰菊酯、氟丙菊酯、苯醚氰菊酯、氟氯氰菊酯、氯氰菊酯、氟氰戊菊酯、氰戊菊酯、氟胺氰菊酯、溴氰菊酯、氯菊酯等16种菊酯残留量的方法。样品经V(丙酮)∶V(乙酸乙酯)∶V(正己烷)=1∶2∶1提取,经GPC去除大分子的色素和类脂杂质,弗罗里硅土SPE柱进一步净化,以毒死蜱同位素D-10作内标,内标法定量。方法的回收率67.2%~108%之间。变异系数小于18%。16种菊酯方法定量限在0.0125~0.025 mg/kg之间。
【基金】十一五课题“农药与兽药残留确证检测技术研究”(2006BAK02A08)项目资助
【DOI】CNKI:SUN:FXSY.0.2009-S1-004
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凝胶过滤色谱-蒸发光散射法监测麦冬多糖色谱分离的研究

【作者中文名】林晓; 姜艳; 徐德生; 冯怡;
【作者单位】上海中医药大学中药现代制剂技术教育部工程研究中心; 上海中医药大学附属曙光医院;
【文献出处】中草药, Chinese Traditional and Herbal Drugs, 编辑部邮箱 2009年 03期 
期刊荣誉:中文核心期刊要目总览  ASPT来源刊  中国期刊方阵  CJFD收录刊
【关键词】麦冬; 多糖; 高效凝胶过滤色谱; 纯化;
【摘要】目的探讨高效凝胶过滤色谱-蒸发光散射检测法(HPGPC-ELSD)用于监测多糖分离纯化的可行性和优点。方法以麦冬多糖为模型多糖,比较DEAE SepharoseTMFast Flow、Sephadex G-50和G-25柱色谱的纯化效果,比较分别以HPGPC-ELSD和传统的蒽酮-硫酸法测定结果为收集标准时的纯化情况。结果通过HPGPC-ELSD测定确知,DEAE Sepharose可将麦冬多糖粗提物中的非中性糖部分除去;Sephadex G-50和G-25均不能够很有效地将粗多糖中的麦冬多糖与低聚糖和单糖分离。结合HPGPC-ELSD和蒽酮-硫酸法的优点,将其合理组合用于监测麦冬多糖的凝胶色谱分离,可以同时确保多糖色谱分离纯化的速度和质量。结论以HPGPC-ELSD测定结果作为收集标准特别适合于较难分离或纯化要求较高的多糖类成分的分离纯化。
【基金】国家中医药管理局中医药科学技术专项(06-07ZQ04);; 上海市青年科技启明星计划(07QA14050);; 上海市教委重点学科资助项目(J50302)
【DOI】CNKI:SUN:ZCYO.0.2009-03-024
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快速溶剂萃取—凝胶渗透色谱净化—GC/MS分析土壤中酞酸酯(PAEs)

【英文篇名】Analysis of Phthalates(PAEs) in Soil Using GC/MS Coupled with Accelerated Solvent Extraction and Gel Permeation Chromatographic Purification
【作者中文名】邵昶铭; 朱文萍;
【作者英文名】SHAO Chang-ming; ZHU Wen-ping(Gansu Environmental Monitoring Center; Lanzhou Gansu 730030; China);
【作者单位】甘肃省环境监测中心站;
【文献出处】干旱环境监测, Arid Environmental Monitoring, 编辑部邮箱 2009年 02期 
期刊荣誉:ASPT来源刊  CJFD收录刊
【关键词】GC/MS选择离子检测; 酞酸酯类化合物; 加速溶剂萃取; GPC净化;
【英文关键词】GC-MS-SIM; phthalates compounds; accelerated solvent extraction; GPC purification;
【摘要】采用毛细管柱气相色谱—质谱选择离子检测技术,结合加速溶剂萃取和凝胶渗透色谱净化方法,分析土壤中的6种酞酸酯类(PAEs)化合物。结果表明,土壤中6种PAEs检出限在14~42μg/kg间,加标平均回收率为65.5%~104.4%,相对标准偏差为5.19%~9.61%。方法具有操作简便、纯化效果好和对环境友好的特点,且具有很强的实用性。
【英文摘要】The analytical method of six types of phthalates(PAEs) compounds in soil using capillary column gas chromatography-mass spectrometry with selected ion monitor(GC-MS-SIM) coupled with accelerated solvent extraction and gel permiation chromatographic purification has been established.The results indicated that the determination limit of six types of PAEs in soil ranged from 14 μg/kg to 42 μg/kg with 65.5%~104.4% average recoveries and 5.19%~9.61% relative standard deviation.The method with the advantages of s...
【DOI】CNKI:SUN:GHJC.0.2009-02-002
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固相萃取-在线凝胶渗透色谱-气相色谱/质谱法测定板栗中44种有机磷农药残留

【英文篇名】Determination of 44 Organophosphorous Pesticides Residual in Chestnut Using Solid Phase Extraction and On-line Gel Permeation Chromatography/Gas Chromatography-Mass Spectrometry
【作者中文名】吴岩; 康庆贺; 高凯扬; 李志斌;
【作者英文名】WU Yan1; KANG Qing-He1; GAO Kai-Yang2; LI Zhi-Bin31(Heilongjiang Entry-Exit Inspection and Quaratine Bureau; Harbin 150001)2(Institute of Chemistry and Materials Science Heilongjiang University; Harbin 150086)3(College of Chemistry; Jilin University; Changchun 130012);
【作者单位】黑龙江出入境检验检疫局; 黑龙江大学化学化工与材料学院; 吉林大学化学院;
【文献出处】分析化学, Chinese Journal of Analytical Chemistry, 编辑部邮箱 2009年 05期 
期刊荣誉:中文核心期刊要目总览  ASPT来源刊  中国期刊方阵  CJFD收录刊
【关键词】固相萃取; 在线凝胶渗透色谱-气相色谱/质谱; 农药多残留; 板栗; 有机磷农药;
【英文关键词】Solid phase extraction; on-line gel permeation chromatography-gas chromatography-mass spectrometry; pesticide residues; chestnut; organophosphorous pesticides;
【摘要】建立了板栗中44种有机磷农药多残留的分析方法。样品以V(乙腈)∶V((水)=4∶1为提取剂,经高速匀浆方法提取,提取液以ENVI-18固相萃取柱净化,除去样品中大部分的脂肪和甾醇等干扰基质,再经在线凝胶渗透色谱-气相色谱/质谱(GPC-GC/MS)分析,进一步除去样液中色素和脂肪等大分子干扰物质,有效地降低了样品中的复杂基质所带来的背景干扰。加标水平为0.05 mg/kg时,大部分农药的回收率为65%~120%,相对标准偏差小于15%;44种农药的检出限为0.002~0.05 mg/kg。采用外标法定量,气相色谱-质谱法(GC-MS)定性定量分析,线性关系和回收率结果均满意。实验证明,本方法是一种快速、准确、灵敏度高的同时检测板栗中有机磷农药多残留的检测方法。
【英文摘要】An analytical method has been developed for the determination of 44 organophosphorous pesticides in chestnut.With acetonitrile-water(4∶1,V/V) as the extraction solution,the samples were extracted by means of high-speed homogenization.And the crude extract was purified by ENVI-18 solid phase extraction column to remove most fats and sterols in samples,then after on-line GPC-GC/MS analysis which further removed macromolecular interference material,such as pigment and fat,the backgroud interference brought abo...
【基金】“十一五”国家科技支撑计划课题(No.2006BAk2A08-12)资助
【DOI】CNKI:SUN:FXHX.0.2009-05-031
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