硫酸庆大霉素中甲醇残留量定量检测气相色谱法的建立

Establishment of a gas chromatography for quantitative measurement of residual methanol in gentamycin sulfate

目的 建立一种顶空进样气相色谱法,以定量检测硫酸庆大霉素中甲醇的残留量. 方法 使用DB-624气相色谱柱,尺寸为20 m（长）×0.53 mm（内径）×3.00 μm（膜厚）.以氮气为载气,流经气化室与气化的甲醇和乙醇混合,然后混合气体进入色谱柱进行分离.甲醇和乙醇气体先后进入氢火焰离子化检测器,在氢火焰作用下化学电离形成离子流,可通过测定离子流强度对其进行检测.结果 甲醇气体与乙醇气体完全分离,在考察范围内有良好的线性,相关系数为0.999 28.甲醇最低检测限为0.40μg/ml,定量限为1.32 μg/ml.甲醇平均回收率为99.99％.两名分析员分别对同一浓度级6个平行测试液检测,测定结果的相对标准偏差为2.7％.结论 建立的方法灵敏度和准确度均达到有机溶剂残留量的检测要求,可用于硫酸庆大霉素中甲醇残留量的定量检测.

Objective To establish a head-space gas chromatography for quantifying residual methanol in gentamycin sulfate.Methods DB-624 chromatographic column （20 m ＆#215; 0.53 mm ＆#215; 3.00μm）and nitrogen （as a carrier gas） were used.The nitrogen was mixed with gasification methanol and ethanol in a gasification chamber.Then,the mixed gas entered the chromatographic column to be separated.Methanol and ethanol gases entered a hydrogen flame ionization detector successively and formed ion current under action of hydrogen flame.They were tested by measurement of intensity of ion current.Results Methanol and ethanol gases were completely separated.A good linearity was observed within the scope of investigation and the correlation coefficient was 0.999 28.The detection and quantification limits of methanol were 0.40 and 1.32 μg/ml,respectively.The average recovery was 99.99%.Six parallels were prepared from methanol solutions of same concentration magnitude and determined independently by two analysts.The relative standard deviation of the results was 2.7%.Conclusions The sensitivity and accuracy of the established method meet the detection requirements of organic solvent residuex The method can be used for quantification of residual methanol in gentamycin sulfate.