顶空气相色谱法测定盐酸罗哌卡因原料药中残留溶剂  

Determination of Residual Solvents in Ropivacaine Hydrochloride by Headspace Gas Chromatography

作　　者：王静文[1] 徐代月 左宁[1] 文强 陈华[1] 尹利辉[1] Wang Jingwen;Xun Daiyue;ZuoNing;Wen Qiang;Chen Hua;Yin Lihui(National Institutes for Food and Drug Control,Beijing 102629,China)

机构地区：[1]中国食品药品检定研究院,北京102629

出　　处：《中国药师》2022年第12期2290-2294,共5页China Pharmacist

摘　　要：目的:建立盐酸罗哌卡因原料药中8种残留溶剂乙醇、丙酮、异丙醇、甲基异丁酮、二氯甲烷、三氯甲烷、溴丙烷、甲苯的顶空气相色谱检测方法。方法:采用DB-624 UI毛细管色谱柱(60 m×0.25 mm, 1.4μm),载气为氮气,样品溶剂为10%二甲亚砜,顶空进样,进样口温度为220℃,程序升温,进样分流比20∶1,氢火焰离子化检测器(FID),检测器温度为280℃。结果:8种残留溶剂在各自的范围内线性关系良好,线性相关系数(r)均>0.994,检测限范围为0.01~0.36 ng,加标回收率在91.1%~111.4%,来自5个厂家的10批样品中8种残留溶剂的含量均未超过限度。结论:该方法合理、准确可行,灵敏度高,专属性强,可以为盐酸罗哌卡因原料药残留溶剂检测提供有力的技术支持。Objective: To develop a headspace GC method for the determination of eight residual solvents in ropivacaine hydrochloride. Methods: A DB-624 UI(60 m×0.25 mm, 1.4 μm)column was used with nitrogen as the carrier gas and 10% DMSO as the sample solvent. Headspace injection was applied with the injection port temperature at 220 ℃ with temperature programming, and the injection split ratio was 20∶1. An FID was used as the detector with the temperature at 280℃. Results: Good linearity was obtained for 8 solvents with the correlation coefficients(r) above 0.994. The limits of detection of the 8 residual solvents were 0.01-0.36 ng and the spiked recoveries were within the range of 91.1%-111.4%. The contents of the 8 residual solvents in 10 batches of samples did not exceed the limits. Conclusion: This method is accurate, sensitive, simple and feasible, and can provide strong technical support for the detection of residual solvents in ropivacaine hydrochloride.

关 键 词：盐酸罗哌卡因原料药 残留溶剂 顶空气相色谱法 人用药品注册技术要求国际协调会 气相色谱-质谱联用仪 

分 类 号：R917[医药卫生—药物分析学]