超高效液相色谱-串联质谱法检测盐酸洛哌丁胺胶囊中混入诺氟沙星的研究  

UPLC-MS in the Detection of Norfloxacin in Loperamide Hydrochloride Capsules

作　　者：张翠英[1] 徐金玲[2] 王雪芹[1] 安华民[1] 

机构地区：[1]河南省食品药品检验所,河南郑州450003 [2]河南中医学院,河南郑州450003

出　　处：《中国药房》2008年第7期538-539,共2页China Pharmacy

摘　　要：目的:建立以超高效液相色谱-串联质谱法检测盐酸洛哌丁胺胶囊中混入诺氟沙星的方法。方法:色谱柱为C18,流动相为乙腈-0.1%甲酸溶液(梯度洗脱),流速为0.3mL.min-1,柱温为35℃,进样量为10μL;离子源为ESI,毛细管电压为3.0kV,离子源温度为110℃,扫描方式为多反应检测。结果:结合液相色谱保留时间(包括紫外光谱)、准分子离子和二级质谱裂解碎片3方面信息分析得出5批样品中有2批混入了诺氟沙星。结论:本方法选择性强、灵敏度高,可用于检测该制剂中是否混入诺氟沙星。OBJECTIVE： To detect whether there is mixing of norfloxacin in loperamide hydrochloride capsules by U-PLC-MS. METHODS： The separation of norfloxacin was performed on C18 column with column temperature set at 35℃, and the mobile phase was composed of acetronitrile and 0.1% formic acid （gradient elution） with a flow rate of 0.3 mL·min^-1. The sample size was 10 μL. ESI source was applied with capillary tube tension at 3.0 kV and ion source temperature at 110 ℃, and scan mode was multiple reaction monitor. RESULTS： It has been proved that there was norfloxacin in 2 of the total 5 batches of samples based on the data of retention time of RP HPLC including ultraviolet spectra, the quasi - molecular ion and the second order mass spectra split fragments. CONCLUSION： The method is highly selective and sensitive, and can be used to detect whether norfloxacin has been illegally added into loperarnide hydrochloride capsules.

关 键 词：盐酸洛哌丁胺胶囊 诺氟沙星 超高效液相色谱-串联质谱法 

分 类 号：R927.2[医药卫生—药学] R975.5