气相色谱法测定3-氯-7-氨基去乙酰氧基头孢烷酸中残留溶剂

Determination of residual solvents in 7-amino-3-chloro cephalosporanic acid by gas chromatography

目的:建立3-氯-7-氨基去乙酰氧基头孢烷酸(7-ACCA)中丙酮、甲醇、二氯甲烷、乙酸乙酯、异丁醇、吡啶、甲苯残留量的测定方法。方法:采用气相色谱法,载气为氮气,FID检测器,色谱柱为Agilent INNOWAX毛细管柱,柱温为程序升温:起始温度70℃,保持6 min,以10℃/min升温至160℃,保持1 min;进样量1.0μl,分流进样,分流比10∶1,外标法检测7-ACCA中丙酮、甲醇、二氯甲烷、乙酸乙酯、异丁醇、吡啶、甲苯的含量。结果:在本研究建立的色谱条件下,丙酮、甲醇、二氯甲烷、乙酸乙酯、异丁醇、吡啶、甲苯的最低检出质量浓度分别为2.5μg/ml、1.5μg/ml、15μg/ml、2.5μg/ml、2.5μg/ml、2.5μg/ml、11μg/ml。样品中仅检测到丙酮,且其残留量远在药典规定的限量以下。结论:建立的方法能有效控制7-ACCA中丙酮、甲醇、二氯甲烷、乙酸乙酯、异丁醇、吡啶、甲苯的残留量。

Objective: To develop a gas chromatography method for determination of residual solvents in 7-amino-3-chloro cephalosporanic acid(7-ACCA).Methods: The residual levels of acetone,methanol,dichloromethane,ethyl acetate,isobutanol,pyridine and toluene in 7-ACCA were measured by gas chromatography using Agilent INNOWAX capillary column(30 m×0.32 mm,0.5 μm).The initial column temperature was 70℃ maintained for 6 min and then raised(10℃/min) to 160℃ for 1 min.Nitrogen gas was used as carrier and FID as detector.T...