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目的:建立奥替溴铵中甲醇、三氯甲烷、环己烷、丙酮、乙酸乙酯5种有机溶剂残留量检测方法。方法:采用顶空气相色谱法,载气为氮气,FID检测器,色谱柱为DB-624毛细管柱,程序升温,外标法测定了奥替溴铵中5种有机溶剂的残留量。结果:5种有机溶剂完全分离,分别在考察浓度3.04～48.64,0.51～8.10,0.40～6.48,4.12～65.92,4.26～68.16μg·ml~(-1)范围内具有良好的线性关系,r分别为0.999 3,0.999 9,0.999 4,0.999 6,0.999 7,平均回收率依次为95.4%,85.2%,83.5%,90.3%,87.3%,RSD分别为2.4%,2.9%,3.5%,2.7%,3.1%(n=9),最低检测限分别为0.12,0.09,0.23,0.04,0.05μg·ml~(-1)。结论:该方法简便、准确,可用于奥替溴铵中几种残留溶剂的同时检测。
OBJECTIVE: To develop a method for the determination of 5 organic solvents, including methanol, trichloromethane, cyclohexane, acetone and ethyl acetate, in Otibromide. Methods: The residues of five organic solvents in Otibromide were determined by headspace gas chromatography, nitrogen as carrier gas, FID detector and DB-624 capillary column. Results: The five organic solvents were completely separated and had good linear relationship in the range of 3.04 ~ 48.64,0.51 ~ 8.10,0.40 ~ 6.48, 4.12 ~ 65.92, 4.26 ~ 68.16μg · ml ~ (-1) The average recoveries were 95.4%, 85.2%, 83.5%, 90.3% and 87.3% respectively, with RSDs of 2.4%, 2.9%, 3.5% and 2.7%, respectively , 3.1% (n = 9), the minimum detection limits were 0.12,0.09,0.23,0.04,0.05μg · ml -1. Conclusion: The method is simple and accurate and can be used for simultaneous determination of several residual solvents in oltipran.