摘要
目的建立顶空气相色谱法测定硫酸氢氯吡格雷中有机溶剂残留量。方法采用Agilent DB-624毛细管柱（30m×0．53mm，3．0μm）；氮气为载气，流速为2．0mL·min^-1；分流比为10：1；进样口温度为200℃；FID检测器，检测器温度为250℃；毛细管柱温度为40℃。顶空进样，平衡温度为80℃，平衡时间为30min；以水为溶剂，外标法测定硫酸氢氯吡格雷中甲醇、丙酮、乙腈、二氨甲烷、乙酸乙酯和仲丁醇的残留量。结果在本文色谱条件下，甲醇、丙酮、乙腈、二氯甲烷、乙酸乙酯和仲丁醇均能得到良好的分离度，空白对照无干扰，检测浓度在所考察的范围内与峰面积具有良好的线性，R^2=0．9988～0．9999；平均回收率为96．6％～102．7％，精密度试验及准确度试验的RSD均小于5．0％，甲醇、丙酮、乙腈、二氯甲烷、乙酸乙酯和仲丁醇检测限分别为1．20，0．32，0．79，0．43，0．32，0．78μg·mL^-1。结论本试验建立的色谱方法简便、准确，灵敏度高，适合硫酸氢氯吡格雷有机溶剂残留量的检测。
Objective To establish a method of headspace gas chromatography for the determination of residual solvents in Clopidogrel Bisulfate. Methods The residual solvents in Clopidogrel Bisulfate were separated by Agilent DB -624 Capillary Column （ 30 m ×0.53mm,3.0μm） with FID detector. The carried gas was N2 , the flow rate was 2.0 mL · min^ - 1 and the split ratio was 10： 1. The injector temperature and the detector temperature were controlled at 200 ℃ and 250 ℃ respectively. The column temperature was controlled at 40 ℃. The water was used as solvent. The temperature of injector in equilibrium was 80 ℃ for 30 min. External standard method was used for the determination of methanol, acetone, acetonitrile, dichloromethane, ethyl acetate and secondary butyl alcohol in Clopidogrel Bisulfate. Results The detected solvents （ methanol, acetone, acetonitrile, dichloromethane, ethyl acetate, secondary butyl alcohol ） were separated completely, blank control had no interference. The calibration curve of each solvent showed a good linear relationship （ R^2 = 0. 998 8 - 0. 999 9 ） with good precision and accuracy （ RSD were less than 5.0% ）. The average recovery rate was in the range of 96.6% - 102.7 %. The detection limit of methanol,acetone, acetonitrile, dichloromethane, ethyl acetate and secondary butyl alcohol were 1.20,0.32,0.79,0.43,0.32,0.78 μg · mL^ - 1. Conclusion The established methed was simple, accurate, sensitive, and can be used for the determination of residual solvents in Clopidogrel Bisulfate.
出处
《齐鲁药事》
CAS
2011年第8期455-457,共3页
qilu pharmaceutical affairs
关键词
硫酸氢氯吡格雷
残留溶剂
顶空气相色谱法
Clopidogrel Bisulfate
Residual solvents
Headspace gas chromatography
