摘要
为检测鱼腥草注射液中非法添加的庆大霉素,建立了以HPLC-ELSD进行初筛,UPLCMS/MS进行确证并定量的系统方法。十八烷基键合硅胶为填充剂,0.2mol/L三氟醋酸-甲醇(92∶8)流动相作为HPLC-ELSD初筛条件。以0.1%甲酸乙腈溶液-0.1%甲酸水溶液(10∶90)为流动相,流速0.3mL/min,在电喷雾离子化电离源上以多反应监测方式进行正离子检测,建立UPLC-MS/MS检测方法,用于定量分析的离子对为m/z478.6→157.1(庆大霉素C_1)。结果表明,庆大霉素C_1在0.15~1.35μg/mL浓度范围内,峰面积与浓度呈良好的线性关系,线性方程为y=5519.3x+879.24,R=0.9965。庆大霉素C_1在鱼腥草注射液中检测限为0.15g/L。
A primary screening method of Gentamicin in Houttuynia Injection was established by high performance liquid chromatography with evaporative light scattering detector （HPLC-ELSD）, using 0.2 mol/L trifluoroacetic acid and methanol （92：8） as the mobile phase. A qualitative and quantitative method of Gentamicin in Houttuynia Injection was established by ultra-high performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS）, using water （0.1% formic acetic） and acetonitrile （0.1% formic acetic） （90：10） as the mobile phase at a flow rate of 0.3 ml/min. At positive electrospray ionization mode, selected reaction monitoring of the precursor-product ion transitions m/z of 478.6→157.1 （C1） for gentamicin. The linear calibration curve of gentamicin was y=5519.3x＋879.24 （R=0.9965）, obtained in a concentration range of 0.15 μg/ml～1.35 μg/ml with a limit of detection of 0.15 g/L in Houttuynia Injection
出处
《中国兽药杂志》
2018年第3期45-51,共7页
Chinese Journal of Veterinary Drug
基金
兽药安全与质量评价技术研究与应用(2015BAD11B03-4)
