顶空毛细管气相色谱法测定马来酸桂哌齐特中的残留溶剂

目的 建立顶空气相色谱法测定马来酸桂哌齐特中二氯甲烷、乙腈、甲苯、吡啶4种有机溶剂残留量的方法。方法色谱柱为HP—FFAP石英毛细管柱，柱温130℃，检测器为FID检测器，检测器温度为250℃，进样口温度为200℃，以水为溶剂。结果二氯甲烷、乙腈、甲苯、吡啶检测浓度的线性范围分别为0．012～0．60（r=0．9999）、0．0082～0．41（r=0．9995）、0．0178—0．89（r=0．9998）、0．004—0．20mg／mL（r=0．9996）；平均回收率为96．6％～99．0％（RSD=1．1％～2．5％）；最低检出限为0．84～9．85μg／mL；3批样品中4种有机溶剂残留量均符合《中国药典》要求。结论该方法简单、准确、灵敏度高、重现性好，可用于该药物中有机溶剂残留量的测定。

Determination of Residual Organic Solvents in Cinepazide Maleate by Capillary Gas Chromatography with Headspace Sampling

Objective To establish a headspace GC method for the determination of residual organic solvents dichloromethane, aeetonitrile, toluene and pyridine in cinepazide maleate. Methods The residual organic solvents were separated on HPFFAP capillary column. FID was used as detector with a temperature of 250℃, the inlet temperature was 200℃, and water as the solvent. Results The linear ranges of dichloromethane, acetonitrile, toluene and pyridine were 0. 012 -0. 60（ r = 0. 999 9）, 0. 008 2 -0. 41 （ r = 0. 999 5）,0.017 8 -0. 89（ r= 0. 999 8）, 0. 004 -0.20 mg/mL（ r =0. 999 6） ,respectively. The average recovery rates were ranged from 96. 6% to 99.0% with RSD ranged at 1.1% - 2. 5%. The detection limits were 0. 84 - 9.85μg/mL. The residual levels for the 4 organic solvents in 3 batches of samples were all up to the standard stipulated in China Pharmacopeia. Conclusion The method is simple, accurate, sensitive and reproducible, which can be used for the determination of the residual organic solvents in cinepazide maleate.