顶空-气相色谱法测定注射用美洛西林钠中的微量二硫化碳  

Determination of the trace of carbon disulfide in melocillin sodium for injection by headspace-gas chromatography

作　　者：肖钦钦 陈希 段和祥 裴昆 章红 Xiao Qinqin;Chen xi;Duan Hexiang;Pei Kun;Zhang Hong(Jiangxi Institute for Drug Control,NMPA Key Laboratory of Quality Evaluation of Traditional Chinese Patent Medicine,Jiangxi Province Engineering Research Center of Drug and Medical Device Quality,Nanchang 330029)

机构地区：[1]江西省药品检验检测研究院,国家药品监督管理局中成药质量评价重点实验室,江西省药品与医疗器械质量工程技术研究中心,南昌330029

出　　处：《中国抗生素杂志》2024年第3期355-359,共5页Chinese Journal of Antibiotics

摘　　要：目的建立注射用美洛西林钠中微量CS_(2)的顶空-气相色谱测定方法。方法采用DB-624(30 m×0.53 mm×3μm)毛细管柱,进样口温度为160℃;起始温度为40℃,维持5 min,再以60℃/min的速率升温至160℃,维持8 min;火焰光度检测器(FPD),加热器和辅助传输线温度为200℃,燃烧室温度为125℃;顶空瓶平衡温度为80℃;平衡时间为30 min。结果CS_(2)在0.04~0.8μg/mL浓度范围内峰面积与浓度呈二次方曲线关系,检测限(LOD)为0.01μg/mL;12家生产企业的157批次样品中87批次样品检出CS_(2),33批次含量超过拟定限度(3.2μg/g),样品中CS_(2)主要由胶塞迁移而来。结论该方法重现性好,准确度高,可用于对本品中微量CS_(2)的检测,为注射剂药品生产企业选择适宜的胶塞提供了质量依据。Objective This study established a method for the determination of CS_(2)in mezlocillin sodium for injection by headspace-gas chromatography.Methods The method was used with the capillary column DB-624(30 m×0.53 mm×3μm)andthe temperature of the injection port was 160℃.The column temperature was programmed(the initial column temperature was 40℃and kept for 5 min at a speed of 60℃/min,until raised to 160℃and kept for 8 min).The sample was detected by a flame photometric detector(FPD)with a heater and auxiliary transmission line temperature of 200℃and a combustion chamber temperature of 125℃.The equilibrium temperature of the headspace bottle was 80℃and the balance time was 30 min.Results The mass concentration of CS_(2)had a quadratic relationship with the peak area in the concentration range of 0.04~0.8μg/mL,and the detection limit(LOD)was 0.01μg/mL.CS_(2)was detected in 87 batches of 157 samples from 12 manufacturing enterprises,and 33 batches of samples exceeded the proposed limit(3.2μg/g).The CS_(2)in the samples was mainly migrated from the rubber plug.Conclusion The method had good reproducibility,high accuracy and could be used for the detection of trace amounts of CS_(2)in this product,which provided a quality basis for the selection of suitable stoppers for injection drug manufacturers.

关 键 词：注射用美洛西林钠 二硫化碳(CS_(2)) 顶空-气相色谱 胶塞 质量控制 

分 类 号：R978.1[医药卫生—药品]