摘要
建立一种超高效液相色谱-串联质谱法测定氨溴特罗口服溶液中1种基因毒性杂质的含量。采用Waters ACQUITY UPLC BEH C18色谱柱,以0.1%甲酸的水溶液为流动相A,乙腈为流动相B,进行梯度洗脱;流速为0.3 mL/min,柱温为30℃;采用电喷雾离子源(ESI),在正离子模式下进行多反应监测(MRM),对氨溴索杂质F进行定量检测。该杂质在0.720 8~36.04 ng/mL范围内有良好的线性关系(R^(2)>0.99),检测限为0.036 04 ng/mL,定量限为0.072 08 ng/mL,加标回收率在99.2%~103.0%,对照品溶液和加标供试品溶液在4℃放置24 h稳定。本方法简便迅速,灵敏度高,专属性好,准确可靠,具有良好的耐用性,可用于测定氨溴特罗口服溶液中氨溴索杂质F的含量,为氨溴特罗口服溶液的质量控制提供技术支撑。
A method based on ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLCMS/MS)was established for the determination of a genotoxic impurity in ambroxol oral solution.Gradient elution was performed on a Waters ACQUITY UPLC BEH C₁₈column,with 0.1%formic acid as mobile phase A and acetonitrile as mobile phase B.The flow rate was set at 0.3 mL/min,and the column temperature was maintained at 30℃.Ambroxol impurity F was quantitatively analyzed via multiple reaction monitoring(MRM)in positive ion mode using an electrospray ionization(ESI)source.The impurity had a good linear relationship in the range of 0.7208 to 36.04 ng/mL(R^(2)>0.99).The limit of detection was 0.03604 ng/mL and the limit of quantitation was 0.07208 ng/mL.The recoveries ranged from 99.2%to 103.0%.The standard solution and spiked test solution remained stable when stored at 4℃for 24 h.This method exhibitsed high sensitivity and specificity,along with simplicity,rapidity,accuracy and reliability,as well as good durability.It can be used for the determination of ambroxol impurity F in ambroxol hydrochloride and clenbuterol hydrochloride oral solutions,providing technical support for quality control.
作者
张银
黄星宇
ZHANG Yin;HUANG Xingyu(SCMPA Key Laboratory for Quality Research and Control of Chemical Medicine,Chengdu Institute for Drug control,Sichuan Chengdu 610045,China)
出处
《广州化工》
2026年第2期118-121,共4页
GuangZhou Chemical Industry
关键词
液相色谱-串联质谱
氨溴特罗口服溶液
基因毒性杂质
氨溴索杂质
UPLC-MS/MS
Ambroxol hydrochloride and Clenbuterol hydrochloride oral solution
Genotoxic impurity
Ambroxol impurity
