毛细管气相色谱法测定羟乙基淀粉中2-氯乙醇的残留量Determination of 2-chloroethanol residue in hydroxyethyl starch by capillary GC
高广慧;王晓黎;董宇;慕善学;廉瑛;
GAO Guang-hui1,WANG Xiao-li1,DONG Yu1,MU Shan-xue2,LIAN Ying3(1.Liaoning Provincial Institute for Food And Drug Control,Shenyang 110023,China;2.Shenyang Pharmaceutical University,Shenyang 110026,China;3.Shenyang Yilian Xin Hai Pharmaceutical Co.,Ltd,Shenyang 110016,China)
摘要(Abstract):
目的建立毛细管气相色谱法测定羟乙基淀粉中2-氯乙醇的残留量。方法采用毛细管气相色谱法。色谱柱为DM-WAX弹性石英毛细管柱(30 m×0.25 mm,0.25μm);载气为氮气;检测器为ECD;进样口和检测器温度均为250℃;柱温为程序升温,初始温度90℃,保持12 min,以每分钟20℃升温至120℃,保持2 min。结果2-氯乙醇质量浓度在14.30119.2μg.L-1内线性关系良好,r=0.997 6;回收率为98.4%(n=9);检测限为9.54×10-3ng;定量限为2.86×10-2ng。结论本法灵敏度高,简单,易行,结果准确可靠,可为羟乙基淀粉的质量控制提供依据。
Objective To establish a GC method for the determination of 2-chloroethanol residue in hydroxyethyl starch.Methods A column of DM-WAX was used with ECD as detector;nitrogen was selected as carrier gas.The injector temperature and the detector temperature were 250 ℃;the programmed column temperature was set at 90 ℃ for 12 min and then to 120 ℃ at the rate of 20 ℃·min-1 followed by holding for 2 min.Results A good linearity was obtained at the concentration of 14.30-119.2 μg·L-1 with correlation of 0.997 6.The average recovery was 98.4%(n=9),the limit of detection was 9.54×10-3 ng;the limit of quantity was 2.86×10-2 ng.Conclusions This method is simple,accurate and feasible.It is very suitable for the quality control of 2-chloroethanol in hydroxyethyl starch.
关键词(KeyWords):
气相色谱法;羟乙基淀粉;2-氯乙醇;溶剂残留
GC;hydroxyethyl starch;2-chloroethanol;residual solvent
基金项目(Foundation):
作者(Authors):
高广慧;王晓黎;董宇;慕善学;廉瑛;
GAO Guang-hui1,WANG Xiao-li1,DONG Yu1,MU Shan-xue2,LIAN Ying3(1.Liaoning Provincial Institute for Food And Drug Control,Shenyang 110023,China;2.Shenyang Pharmaceutical University,Shenyang 110026,China;3.Shenyang Yilian Xin Hai Pharmaceutical Co.,Ltd,Shenyang 110016,China)
DOI: 10.14066/j.cnki.cn21-1349/r.2010.05.017
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- 高广慧
- 王晓黎
- 董宇
- 慕善学
- 廉瑛
GAO Guang-hui1- WANG Xiao-li1
- DONG Yu1
- MU Shan-xue2
- LIAN Ying3(1.Liaoning Provincial Institute for Food And Drug Control
- Shenyang 110023
- China
- 2.Shenyang Pharmaceutical University
- Shenyang 110026
- China
- 3.Shenyang Yilian Xin Hai Pharmaceutical Co.
- Ltd
- Shenyang 110016
- China)
- 高广慧
- 王晓黎
- 董宇
- 慕善学
- 廉瑛
GAO Guang-hui1- WANG Xiao-li1
- DONG Yu1
- MU Shan-xue2
- LIAN Ying3(1.Liaoning Provincial Institute for Food And Drug Control
- Shenyang 110023
- China
- 2.Shenyang Pharmaceutical University
- Shenyang 110026
- China
- 3.Shenyang Yilian Xin Hai Pharmaceutical Co.
- Ltd
- Shenyang 110016
- China)