论文部分内容阅读
目的建立顶空气相色谱法测定罗库溴铵中甲醇、正戊烷、乙醚、丙酮、乙腈、二氯甲烷、乙酸乙酯、乙酸异丁酯8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、正戊烷、乙醚、丙酮、乙腈、二氯甲烷、乙酸乙酯、乙酸异丁酯的检测浓度的线性范围分别为0.06～3.00(r=0.9999)、0.01～2.0(r=0.9999)、0.01～2.0(r=0.9998)、0.01～2.0(r=0.9999)、0.0082～0.4100(r=0.9998)、0.012～0.600(r=0.9998)、0.01～2.0(r=0.9999)、0.01～2.0mg·mL-1(r=0.9999);平均回收率为97.1%～99.6%(RSD=1.1%～2.2%);最低检出限为0.15～6.44μg·mL-1;3批样品中8种有机溶剂残留量均符合中国药典2005年版的要求。结论本方法简单、准确、灵敏度高、重复性好,可用于该药物中有机溶剂残留量的测定。
OBJECTIVE To establish a method for the determination of residues of eight kinds of organic solvents in methanol, n-pentane, diethyl ether, acetone, acetonitrile, dichloromethane, ethyl acetate and isobutyl acetate in rocuronium by headspace gas chromatography. Methods The column was DB-624 quartz capillary column. The temperature of the column was raised by temperature. The detector was FID detector. The detector temperature was 250 ℃ and the inlet temperature was 150 ℃. The water was used as the dissolution medium. Results The linear ranges of methanol, n-pentane, ether, acetone, acetonitrile, dichloromethane, ethyl acetate and isobutyl acetate were 0.06-3.00 (r = 0.9999) and 0.01-2.0 , 0.01 ~ 2.0 (r = 0.9998), 0.01 ~ 2.0 (r = 0.9999), 0.0082 ~ 0.4100 (r = 0.9998), 0.012 ~ 0.600 · ML -1 (r = 0.9999). The average recoveries ranged from 97.1% to 99.6% (RSD = 1.1% -2.2%). The lowest detection limit was 0.15-6.44 μg · mL -1. Residues are in line with the Chinese Pharmacopoeia 2005 edition of the requirements. Conclusion The method is simple, accurate, sensitive and reproducible. It can be used to determine the residual amount of organic solvents in this medicine.