【摘要】 目的:建立顶空气相色谱法,测定硫酸氢氯吡格雷中丙酮、异丙醇、乙腈、二氯甲烷和乙酸乙酯5种残留溶剂方法。方法 :采用DB-624(6%-氰丙基苯-94%-二甲基硅氧烷共聚物,30m×0.53mm,df=3.0μm)毛细管柱,检测器:FID;温度:250℃;气化室温度:220℃;载气:氮气;流速:4.0m L/min;程序升温:40℃,保持8min,以80℃/min的速度升至200℃保持3min。结果:此色谱条件下,5种溶剂均能得到良好的分离,空白对照无干扰。丙酮、异丙醇和乙酸乙酯在浓度0.25~0.7250mg/m L(r=0.9999、r=0.9985、r=0.9976)范围内,二氯甲烷在浓度0.03~0.0870mg/m L(r=0.9989)范围内,乙腈在浓度0.0205~0.0595mg/m L(r=0.9965)范围内,线性关系良好。平均回收率(n=9)分别为丙酮99.57%(RSD=3.86%)、异丙醇100.03%(RSD=4.38%)、乙腈105.11%(RSD=3.32%)、二氯甲烷99.99%(RSD=3.01%)、乙酸乙酯99.71%(RSD=3.19%)。结论 :方法测定结果准确,灵敏简便,可有效检测硫酸氢氯吡格雷中有机溶剂残留量。更多还原

【Abstract】 Objective: To establish a method of headspace gas chromatography for the determination of fi ve organic residual solvents(acetone, isopropanol, acetonitrile, methylene chloride and ethyl acetate) in Clopidogrel Bisulfate. Methods: A capillary GC method was established with FID detector, using the DB-624(6%-94% cyanide propylbenzene-dimethylsiloxane copolymer, 30m×0.53 mm, df=3.0μm) capillary column. The injector temperature and the detector temperature were controlled at 220℃ and 250℃ respectively. The carried gas was N2, the fl ow rate was 4.0m L/min. The column temperature is initially maintained at 40℃for 8min and then up to 200℃ at the rate of 80℃/min for 3min. Results: The detected fi ve solvents were separated completely, blank control had no interference. The peak area and concentration of acetone, isopropyl alcohol and ethyl acetate showed a good linearity within the concentration range of 0.25~0.7250mg/m L(r=0.9999、r=0.9985、r=0.9976. The peak area and concentration of methylene chloride showed a good linearity within the concentration range of 0.03~0.0870mg/m L(r=0.9989) the peak area and concentration of acetonitrile showed a good linearity within the concentration range of 0.0205~0.0595mg/m L(r=0.9965). The average recovery of acetone, isopropanol, acetonitrile, methylene chloride, ethyl acetate was calculated as 99.57%(RSD=3.86%), 100.03%(RSD=4.38%), 105.11%(RSD=3.32%), 99.99%(RSD=3.01%), 99.71%(RSD=3.19%) respectively(n=9). Conclusion: This method is accurate, sensitive and simple, and can be effectively used in the determination of residual organic solvents in Clopidogrel Bisulfate.更多还原