IR-UPLC-MS/MS法鉴别妇炎康胶囊中非法添加的诺氟沙星

Determination of Norfloxacin illegally added into Fuyankang Capsule by IR-UPLC-MS/MS

目的:建立快速鉴别妇炎康胶囊中非法添加诺氟沙星的方法。方法:采用红外光谱扫描法作为预实验,UPLC-MS/MS法进一步确认诺氟沙星。液质条件为色谱柱C18(2.1 mm×50 mm,1.7μm),流动相为0.1%甲酸水溶液-0.1%甲酸乙腈溶液(梯度洗脱),流速为0.4 mL.min-1,柱温为40℃,进样体积为5μL,离子源为电喷雾离子化源(ESI),毛细管电压为3.5 kV,离子源温度为120℃,在正离子条件下以多反应监测(MRM)方式进行扫描。结果:结合红外光谱、超高效液相色谱保留时间、紫外光谱、准分子离子和二级质谱裂解碎片等方面信息分析得出妇炎康胶囊中非法添加有诺氟沙星。结论:本方法简单快速,选择性强,灵敏度高,结果准确可靠,可用于妇炎康胶囊中非法添加诺氟沙星的定性鉴别。

Objective： An IR-UPLC-MS/MS method was established to detect Norfloxacin illegally added into Fuyankang Capsule rapidlly. Methods： The method of Infrared spectrometry was used as a pretest, then the method of UPLC-MS/MS was used to identify Norfloxacin further more. The separation of Norfloxacin was performed on C18 column with column temperature set at 40℃, and the mobile phase was composed of acetonitrile contained 0. 1% formic acid and water contained 0. 1% formic acid （ gradient elution） with a flow rate at 0. 4 mL · min^-1. The injection volume was 5 μL. ESI source was applied with capillary tube tension at 3.5 kV and ion source temperature at 120℃, and multiple reation monitoring was performed in the positive ion mode. Results ： It has been proved that there was Norfloxacin illegally mixed in Fuyankang Capsule based on the data of the infrared spectrum, the retention time of UPLC in- cluding ultraviolet spectra, the quasi-molecular ion and the second order mass spectra split fragments. Conclusion： The method was highly selective and sensitive, and can be used to detect whether Norfloxacin has been illegally added into Fuyankang Capsule simply and rapidly.