摘要
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 capillary 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 a DB - 624 capillary column using temperature programming. FID was used as detector with a temperature of 250 ℃ ,the inlet temperature was 135 ℃ ,and N,N-dimethyl formamide as the solvent. RESULTS The linear ranges of methanol, pentane, ethyl ether, acetone, acetonitrile, dichloromethane, ethyl acetate and isobutyl acetate were 0. 06 - 3.00 （r =0. 999 9） ,0. 1 -5.0（ r =0. 999 9）, 0. 1 -5.0 （r = 1. 000 0） ,0. 1 -5.0 （r = 1. 000 0） ,0. 008 2 -0. 410 0（r =0. 999 9） ,0. 012 -0. 600（r =0. 999 9）, 0. 1 -5.0 （r =0. 999 9） ,0. 1 -5.0 g·L^-1 （r =0. 999 9）, respectively. The average recoveries were ranged from 96. 6% to 99.4% with RSD ranged of 0. 9% -2. 5%. The detection limits were 0. 61 - 1.74 ng. The residual levels for the eight organic solvents in 3 batches samples were all up to the standard stipulated in China Pharmacopeia. CONCLUSION The method is simple, accurate, sensitive and reproducible, it can be used for the determination of the residual organic solvents in rocuronium bromide.
出处
《中国药学杂志》
CAS
CSCD
北大核心
2010年第7期553-555,共3页
Chinese Pharmaceutical Journal
关键词
罗库溴铵
有机溶剂残留量
毛细管气相色谱法
rocuronium bromide
residual organic solvents
capillary gas chromatography
