顶空毛细管气相色谱法测定盐酸莫雷西嗪中残留溶剂的含量

目的建立顶空气相色谱法测定盐酸莫雷西嗪中甲醇、乙醇、异丙醇、二氯甲烷、乙酸乙酯、四氢呋喃、甲苯7种有机溶剂残留量的方法。方法色谱柱为DB-624石英毛细管柱,柱温采用程序升温,检测器为FID检测器,检测器温度为250℃,进样口温度为150℃,以水为溶解介质。结果甲醇、乙醇、异丙醇、二氯甲烷、乙酸乙酯、四氢呋喃、甲苯的质量浓度的线性范围分别为12.0~240 mg.L-1(r=1.000 0)、10.0~200 mg.L-1(r=0.999 9)、10.0~200 mg.L-1(r=0.999 9)、1.20~24 mg.L-1(r=0.999 9)、10.0~200 mg.L-1(r=0.999 9)、1.44~28.8 mg.L-1(r=0.999 8)、1.78~35.6 mg.L-1(r=0.999 7);平均回收率为98.1%~99.5%(RSD=0.6%~1.7%);定量限为0.22~11.91 mg.L-1;3批样品中7种有机溶剂残留量均符合《中华人民共和国药典》要求。结论本方法简单、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 the contents of residual organic solvents in moracizine hydrochloride by capillary gas chromatography with headspace sampling

Objective To establish a headspace GC method for the determination of residual organic solvents-methanol,alcohol,isopropyl alcohol,dichloromethane,ethyl acetate,tetrahydrofuran,and methylbenzene in moracizine hydrochloride.Methods The residual organic solvents were separated on DB-624 capillary column using temperature programming.FID was used as detector with a temperature of 250 ℃,the inlet temperature was 150 ℃,and water as the solvent.Results The linear ranges of methanol,alcohol,isopropyl alcohol,dichloromethane,ethyl acetate,tetrahydrofuran,and methylbenzene were 12.0-240 mg·L-1(r=1.000 0),10.0-200 mg·L-1(r=0.999 9),10.0-200 mg·L-1(r=0.999 9),1.20-24 mg·L-1(r=0.999 9),10.0-200 mg·L-1(r=0.999 9),1.44-28.8 mg·L-1(r=0.999 8),1.78-35.6 mg·L-1(r=0.999 7),respectively.The average recoveries were ranged from 98.1% to 99.5% with RSD ranged at 0.6%-1.7%.The determination limits were 0.22-11.91 mg·L-1.The residual levels for the seven organic solvents in 3 batches samples met standard that stipulated in China pharmacopeia.Conclusions The method is simple,accurate,sensitive and reproducible;it can be used for the determination of the residual organic solvents in moracizine hydrochloride.