顶空气相色谱法检测血塞通分散片中有机溶剂残留量

Determination of Residual Organic Solvents in Xuesaitong Dispersible Tablets by Headspace Gas Chromatography

目的建立测定血塞通分散片中6种有机溶剂残留量的顶空气相色谱法。方法色谱柱采用以聚乙二醇为固定相的HP-INNOWAX毛细管色谱柱(30 m×0.32 mm,0.25μm);氢火焰离子化检测器(FID);柱温采用程序升温,初始温度为60℃,保持1 min,再以5℃/min升温至100℃,保持13 min,再以20℃/min的速度升温至200℃,保持2 min;进样口温度为240℃;检测器温度为300℃;载气为氮气;流速为2.5 mL/min。顶空进样,顶空瓶平衡温度为70℃,平衡时间为30 min。结果正己烷、甲苯、对二甲苯、邻二甲苯、苯乙烯、1,2-二乙基苯的检测质量浓度线性范围分别为1.014~16.224,1.060~16.960,1.610~18.576,1.169~18.704,0.985~15.760,1.129~18.064μg/mL,相关系数r分别为0.999 6,0.999 9,0.999 9,0.999 6,0.999 4,0.999 2(n=5);回收率均在97.14%~98.73%(n=9);理论板数均大于10 000,相邻峰的分离度均在2.0以上。结论该方法样品处理简单,检测准确,灵敏度高,重复性好,排除了辅料的干扰,可作为血塞通分散片中有机溶剂残留量的考察方法。

Objective To establish the headspace gas chromatography method for determination of six residual organic solvent in Xuesaitong Dispersible Tablets. Methods The chromatographic column adopted HPINNOWAX capillary column with polyethylene glycol as stationary phase（30 m×0.32 mm,0.25μm）, and the FID was used. The column temperature was programmed by heating： the initial temperature was 60 ℃, keep for 1 min, then the temperature was increased to 100 ℃ at 5 ℃/min, keep for 13 min, and then increase to 200 ℃ at 20 ℃/min, keep for 2 min. The inlet temperature was 240 ℃, the detector temperature was 300 ℃, the carrier gas was nitrogen, the flow rate was 2.5 mL/min. Headspace sampling was adopted, headspace equilibrium temperature was 70℃, and equilibrium time was 30 min. Results The concentration linear range of hexane, toluene, p-xylene, o-xylene, styrene, 1, 2-diethylbenzene were 1. 014 - 16. 224, 1. 060 - 16. 960, 1. 610 - 18. 576, 1. 169 - 18. 704, 0. 985 - 15. 760, 1. 129 - 18. 064 g/mL, respectively, and the relative conditions of r were 0. 999 6, 0. 999 9, 0. 999 9, 0. 999 6, 0. 999 4, 0. 999 2, respectively. The recovery rates were 97. 14% - 98.73% （n =9）. The theoretical plates were larger than 10 000, and the separation degree of adjacent peaks was above 2.0. Conclusion The method has simple sample processing, accurate detection, high sensitivity and good reproducibility, and excludes the interference of excipients, which can be used as an investigation method for the determination of residual organic solvents in Xuesaitong Dispersible Tablets.