顶空毛细管气相色谱法测定罗库溴铵中的残留溶剂

Determination of Residual Organic Solvents in Rocuronium Bromide by Capillary Gas Chromatography with Headspace Sampling

关键词:  罗库溴铵  顶空毛细管气相色谱法  残留溶剂

Key words:  rocuronium bromide  headspace capillary gas chromatography  residual organic solvents

摘要:

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=0.999 9)、0.01～2.0(r=0.999 9)、0.01～2.0 (r=0.999 8)、0.01～2.0 (r=0.999 9)、0.008 2～0.410 0(r=0.999 8)、0.012～0.600(r=0.999 8)、0.01～2.0 (r=0.999 9)、0.01～2.0 mg·mL-1 (r=0.999 9)；平均回收率为97.1%～99.6%(RSD=1.1%～2.2%)；最低检出限为0.15～6.44 μg·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

Abstract:

OBJECTIVE To establish a headspace GC method for the determination of residual organic solvents-methanol, pentane, ethyl ether, acetone, acetonitrile, dichloromethane, ethyl acetate and isobutyl acetate in rocuronium bromide. 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, pentane, ethyl ether, acetone, acetonitrile, dichloromethane, ethyl acetate and isobutyl acetate were respectively 0.06-3.00 (r=0.999 9)，0.01-2.0(r=0.999 9)，0.01-2.0 (r=0.999 8)，0.01-2.0 (r=0.999 9 )，0.008 2-0.410 0 (r=0.999 8)，0.012-0.600(r=0.999 8)，0.01-2.0 (r=0.999 9)，0.01-2.0mg·mL-1 (r=0.999 9). The average recoveries were ranged from 97.1% to 99.6% with RSD ranged from 1.1% to 2.2%. The detection limits were 0.15-6.44 μg·mL-1. The residual levels for the eight organic solvents in 3 batches samples were all up to the standard stipulated in Ch.P(2005). CONCLUSION The method is simple, accurate, sensitive and reproducible. It can be used for the determination of the residual organic solvents in rocuronium bromide.