摘要
建立高效液相色谱-质谱联用的方法测定替加环素中遗传毒性杂质9-硝基米诺环素。方法:选用C 18色谱柱(Welch XB-C 18,4.6×50 mm,5μm),以0.1%甲酸(v/v)为流动相:乙腈为流动相,流速为每分钟0.5 mL,进行线性梯度洗脱;质谱条件:采用电喷雾离子源(ESI),多级反应监测(MRM),正离子扫描模式,干燥气温度为300℃,干燥气流速为8 L/min,雾化气压力为35 psi,鞘流气温度为350℃,鞘流气流速为11 L/min,毛细管端电压为3500 V,喷嘴正电压为500 V,喷嘴负电压为1000 V。离子碰撞能为34 V,扫描时间为500 ms,用于定量分析的MRM离子对为m/z→503.2/153.9。该方法在0.0125~0.9580μg·mL^(-1)的范围内线性良好(0.9999),定量限和检出限分别为0.0125和0.0067μg·mL^(-1),方法回收率94.4%~100.8%之间,稳定性较好。本研究所建立的方法快速、灵敏、专属性强,适用于替加环素中基因毒性杂质9-硝基米诺环素的测定。
To establish a LC-MS/MS method for the determination of the residual quantity of potential genetoxic impurity 9-nitrominocycline in tigecycline.The chromatographic conditions were as follows:a Welch ZORBAX XB-C 18(4.6×50 mm,5μm)column using acetonitrile-water(containing 0.1%formic acid)as the mobile phase in gradient elution.The flow rate was 0.5 mL·min-1.The mass spectrometry conditions were as follows:electrospray ionization source(ESI),multistage reaction monitoring(MRM),positive ion scanning mode,ion spray voltage of 3500 V,ion source temperature of 300℃,Sheath Gas Temp of 350℃,Sheath Gas Flow of 11 L/min,ion collision energy of 34 V and scan time of 500 ms.The MRM ion pair for quantitative analysis was m/z→503.2/153.9.The linear range of 9-nitrominocycline was 0.0125~0.9580μg·mL^(-1)(r=0.9999).The limit of detection was 0.0067μg·mL^(-1) and the limit of quantitation was 0.0125μg·mL^(-1).The average recovery was 94.4%~100.8%.The method is simple,rapid and accurate,and can be used for the quality control of 9-nitrominocycline in tigecycline.
作者
易芬芬
邵婷婷
徐慧娟
Yi Fenfen;Shao Tingting;Xui Huijuan(Hanhui-Pharma,Shanghai 200032,China)
出处
《山东化工》
CAS
2021年第19期126-128,131,共4页
Shandong Chemical Industry
