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. The flow of carrier was 1. 0 ml/min, the temperature of injection port and detector was 200℃ and 250℃, respectively. Results: The limits of detection for acetone, methanol, dichloromethane, ethyl acetate, isobutanol, pyridine, toluene in 7-ACCA were 2.5 μg/ml, 1.5 μg/ml, 15 μg/ml,2.5 μg/ml,2.5 μg/ml,2.5 μg/ml and 11 μg/ml, respectively. Only acetone was detected in the sample, and was less than the limits of Ch. P. Conclusion: The method can effectively detect the residual solvents in 7-ACCA.%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2.5 μg/ml、1.5μg/ml、15 μg/ml、2.5μg/ml、2.5μg/ml、2.5 μg/ml、11 μg/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.
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