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顶空-气相色谱法测定止血微球中环氧氯丙烷残留量 被引量:6

Determination of Residue of Epichlorohydrinin Hemostatic Microspheres by Headspace-Gas Chromatography
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摘要 将0.15 g止血微球粉末样品和5.00 mL水置于20 mL顶空瓶中,立即密封顶空瓶,在顶空平衡温度为80℃,平衡时间为30 min的条件下进行顶空采样.以DB-5毛细管柱为固定相,采用电子俘获检测器(ECD),用气相色谱法测定其中环氧氯丙烷残留量.结果表明,环氧氯丙烷的质量浓度在0.02~2.0 mg·L^(-1)内与其峰面积呈线性关系,测定下限(10S/N)为0.005 mg·L^(-1).按标准加入法进行回收试验,回收率为95.3%~101%,测定值的相对标准偏差(n=6)小于7.0%. The powdersample of hemostatic microspheres(0.15 g)and 5.00 mL of water weretakeninto a 20 mL-headspaceflask.The headspaceflask was then sealed hermetically and the headspace-sampling was carried outat80℃for30 min.DB-5 capillarycolumn was used as the stationary phase,electron capture detector(ECD)was adopted for detection of response signals,and residue of epichlorohydrin was determined by headspace-gas chromatography.Asshownbytheresults,linearrelationship betweenvaluesofpeakareaand massconcentrationof epichlorohydrin was obtainedintherange of 0.02-2.0 mg·L^(-1),with lowerlimit of determination(10S/N)of 0.005 mg·L^(-1).Testforrecovery was made by standard addition method,giving resultsinthe range of 95.3%-101%,with RSDs(n=6)ofthe determined valueslessthan7.0%.
作者 李亚利 王宝群 林莎莎 邹圣灿 LI Yali;WANG Baoqun;LIN Shasha;ZOU Shengcan(Qingdao Chen Lan Marine Biological Engineering Co.,Ltd.,Qingdao 266000,China)
出处 《理化检验(化学分册)》 CAS CSCD 北大核心 2022年第3期333-335,共3页 Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
关键词 顶空-气相色谱法 环氧氯丙烷 止血微球 headspace-gas chromatography epichlorohydrin hemostatic microsphere
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