论文部分内容阅读
目的建立毛细管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135℃,以N,N-二甲基甲酰胺为溶剂。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)、0.1～5.0(r=0.9999)、0.1～5.0(r=1.0000)、0.1～5.0(r=1.0000)、0.0082～0.4100(r=0.9999)、0.012～0.600(r=0.9999)、0.1～5.0(r=0.9999)、0.1～5.0g.L-1(r=0.9999);平均回收率为96.6%～99.4%(RSD=0.9%～2.5%);最低检出限为0.61～1.74ng;3批样品中8种有机溶剂残留量均符合《中国药典》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。
OBJECTIVE To establish a method for the determination of residues of 8 organic solvents in methanol, n-pentane, diethyl ether, acetone, acetonitrile, dichloromethane, ethyl acetate and isobutyl acetate in rocuronium by capillary 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 temperature of the detector was 250 ℃ and the temperature of the inlet was 135 ℃. The column temperature was set at N, N-dimethylformamide Solvent. 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 0.1-5.0 , 0.1-5.0 (r = 1.0000), 0.1-5.0 (r = 1.0000), 0.0082-0.4100 (r = 0.9999), 0.012-0.600 (r = 0.9999), 0.1-5.0 -1 (r = 0.9999). The average recoveries ranged from 96.6% to 99.4% (RSD = 0.9% -2.5%). The minimum detectable limit was 0.61 ~ 1.74 ng. Chinese Pharmacopoeia "requirement. Conclusion The method is simple, accurate, sensitive and reproducible. It can be used to determine the residual amount of organic solvents in the drug.