顶空气相色谱法同时测定注射用七叶皂苷钠中8种残留溶剂  

Determination of 8 Residual Solvents in Sodium Aescinate for Injection by HS-GC

作　　者：黄翰林 漆欣筑 祝晶[1] 许波[1] Huang Hanlin;Qi Xinzhu;Zhu Jing;Xu Bo(Guizhou Institute for Food and Drug Control,Guiyang 550004,China)

机构地区：[1]贵州省食品药品检验所,贵州贵阳550004

出　　处：《广东化工》2023年第13期191-193,共3页Guangdong Chemical Industry

基　　金：贵州省科技厅2021年基础研究计划:番茄红素抗氧化应激效应对前列腺癌根治术后阴茎康复的影响及机制研究(黔科合基础-ZK[2021]一般382)。

摘　　要：目的:建立顶空气相色谱法同时测定注射用七叶皂苷钠中甲醇、乙醇、乙酸乙酯、氯苯、甲苯、环己烷、三氯甲烷和苯等8种残留溶剂的残留量,并使用该方法测定9个不同厂家的26批次注射用七叶皂苷钠以及3个不同生产厂家的3批次七叶皂苷钠原料药中的残留溶剂。方法:以6%氰丙基苯和94%二甲基硅氧烷为固定液的毛细管柱为色谱柱,起始温度为40℃,维持8 min,以每分钟8℃的速率升至120℃,维持10 min;进样口温度为220℃;检测器温度为220℃;顶空平衡温度为80℃;平衡时间为45 min。结果:8种有机溶剂之间能有效分离,甲醇、乙醇、乙酸乙酯、氯苯、甲苯、环己烷、三氯甲烷和苯在20~50 mg/mL线性范围内线性关系良好(r≥0.9980);回收率为81.8%~103.1%,RSD(n=6)为1.4%~3.2%;定量限为0.5~58.3μg/mL。26批样品中均未检出甲醇、三氯甲烷和苯,部分注射用七叶皂苷钠检出乙醇、乙酸乙酯、环己烷、甲苯和氯苯,但检出量均远低于规定限度;三批次原料药中存在乙醇、乙酸乙酯和氯苯三种残留溶剂。结论:该方法检测简便、专属性强、检测灵敏度高、各溶剂之间分离效果好,可用于同时测定注射用七叶皂苷钠中8种残留溶剂的残留量。Objective:To establish a headspace gas chromatography method for simultaneous determination of 8 residual solvents in Sodium Aescinate for Injection,and determine 8 residual solvents in 26 batches of Sodium Aescinate for Injection from 9 different manufacturers and 3 batches of Sodium Aescinate API from 3 different manufacturers.Methods:Chromatographic Column with 6%cyanopropylbenzene and 94%dimethylsiloxane as the stationary liquid,the initial temperature is 40℃,and maintained for 8 minutes,and raised to 120℃at the rate of 8℃per minute,and maintained for 10 minutes.The injector temperature is 220℃,the detector temperature is 220℃,the equilibrium temperature of the sample bottle is 80℃and the balance time of the sample bottle is 45 min.Results:Under the selected experimental method,the resolution between the solvent peaks meets the requirements.Methanol,ethanol,ethyl acetate,chlorobenzene,toluene,cyclohexane,trichlormethane and benzene have good linear relationship between 20~50 mg/mL(r≥0.9980),and the average recovery was 81.8%~103.1%,RSD(n=6)1.4%~3.2%,and the quantitative limit is 0.5~58.3μg/mL.And methanol,chloroform and benzene were not detected in 26 batches Sodium Aescinate,but there are 3 residual solvents,ethanol,ethyl acetate and chlorobenzene were detected in the3 batches of API.Conclusion:The method has the advantages of simple detection,strong specificity,high detection sensitivity and good separation effect between solvents.It can be used for the determination of 8 residual solvents in Sodium Aescinate at the same time.

关 键 词：注射用七叶皂苷钠 残留溶剂 顶空气相色谱法 

分 类 号：R917[医药卫生—药物分析学]