顶空进样-气相色谱法检测达托霉素中残留溶剂  

Detection of Residual Solvents in Daptomycin by Headspace Gas Chromatography

作　　者：李佳蕊 韩彬 张雪霞[3] 任凤芝[3] 徐艳梅 闫凯 王巧[2] 高燕霞 LI Jiarui;HAN Bin;ZHANG Xuexia;REN Fengzhi;XU Yanmei;YAN Kai;WANG Qiao;GAO Yanxia(Hebei Institute for Drug and Medical Device Control,Shijiazhuang,Hebei,China 050021;School of Pharmacy,Hebei Medical University,Shijia-zhuang,Hebei,China 050017;North China Pharmaceutical Group New Drug Research and Development Co.,Ltd.,Shijiazhuang,Hebei,China 050021)

机构地区：[1]河北省药品医疗器械检验研究院,河北石家庄050021 [2]河北医科大学药学院,河北石家庄050017 [3]华北制药集团新药研究开发有限责任公司,河北石家庄050021

出　　处：《中国药业》2024年第12期66-69,共4页China Pharmaceuticals

基　　金：河北省自然科学基金[B2022329002]。

摘　　要：目的建立测定达托霉素中3种有机溶剂残留量的顶空进样-气相色谱法。方法色谱柱为Agilent DB-624毛细管柱(60 m×0.53 mm,3.0µm),载气为氮气(流速为5.0 mL/min),程序升温,氢火焰离子化检测器(FID)检测,进样口温度为200℃,检测器温度为230℃,分流比为5∶1(V/V),顶空瓶平衡温度为85℃,平衡时间为30 min,进样量为1µL。结果乙醇、异丙醇和正丁醇质量浓度均在10~200µg/mL范围内与峰面积线性关系良好(r=1.0000);检测限分别为0.75,0.30,0.75µg/mL,定量限分别为2.50,1.01,2.50µg/mL;精密度、稳定性、重复性试验结果的RSD均小于2.0%;平均回收率分别为101.85%,101.65%,102.33%,RSD分别为0.59%,0.77%,0.78%(n=9)。结论该方法专属性强,灵敏度高,精密度好,可用于达托霉素中前述3种有机溶剂残留量的测定。3批样品中检出的有机溶剂残留量远低于国家标准限度。Objective To establish a headspace gas chromatography method for the determination of three organic solvent residues in daptomycin.Methods The chromatographic column was the Agilent DB-624 capillary column(60 m×0.53 mm,3.0µm),the carrier gas was nitrogen with a flow rate of 5.0 mL/min,the temperature was programmed,the flame ionization detector(FID)was adopted,the inlet temperature was 200℃,the detector temperature was 230℃,the split ratio was 5∶1(V/V),the balance temperature of headspace bottle was 85℃,the balance time was 30 min,and injection volume was 1µL.Results The linear ranges of ethanol,isopropanol and n-butanol were 10-200µg/mL(r=1.0000).The limits of detection(LOD)of the above three components were 0.75,0.30,0.75µg/mL,and their limits of quantification(LOQ)were 2.50,1.01,2.50µg/mL,respectively.The RSDs of precision,stability,and repeatability tests were all lower than 2.0%.The average recovery rates of the above three components were 101.85%,101.65%,102.33%,with the RSDs of 0.59%,0.77%,0.78%respectively(n=9).Conclusion This method is specific,sensitive and precise,which can be used for the determination of the above three organic solvent residues in daptomycin.The residual amount of organic solvents detected in three batches of samples is far below the limit of national standard.

关 键 词：达托霉素 冻干工艺 有机溶剂残留 溶解性 复溶时间 

分 类 号：R917[医药卫生—药物分析学]