高效液相色谱－串联质谱法快速测定麻杏石甘口服液中喹诺酮类、磺胺类等17种药物

Rapid Determination of 17 Compouds in Maxingshigan Oral Liquid by UPLC-MS/MS

关键词:  麻杏石甘口服液  超高效液相色谱－串联质谱法  喹诺酮类  磺胺类

Key words:  Maxingshigan oral liquid  UPLC-MS/MS  Qinolones  Sulfonamides

摘要:

建立了麻杏石甘口服液中喹诺酮类、磺胺类等17种药物的高效液相色谱－串联质谱法的快速筛查与定量方法。样品经甲醇超声提取，HLB小柱净化，0.1%甲酸溶解定容后经LC-MS/MS测定。采用 C18色谱柱分离，以乙腈-0.1%甲酸为流动相，梯度洗脱方式；质谱采用电喷雾正离子模式和负离子模式离子化，多反应监测模式(MRM)，外标法标准曲线定量。各待测化合物在各自浓度范围内线性关系良好，相关系数r均大于 0.99。喹乙醇检出限为 10 ng/mL，定量限为25 ng/mL，剩余16种化合物的检出限为5 ng/mL，定量限为 10 ng/mL。各化合物在10、25、50 ng/mL(喹乙醇添加浓度为25、50、100 ng/mL)3个浓度水平下平均回收率在73.87%～116.43%之间，RSD为1.25～8.44%。该方法简便快捷、准确度和灵敏度高，能满足麻杏石甘口服液中17种药物进行快速筛查和准确定量。

Abstract:

A rapid screening and quantification method for 17 compounds such as quinolones, sulfonamides et al in Maxingshigan Oral Liquid was established by UPLC-MS/MS. The samples were ultrasonically extracted with methanol. The extraction cleaned up with a HLB SPE cartridge was determined by liquid chromatography-tandem mass spectrometry in positive and negative ionization mode using an electrospray ionization source with the multiple reaction monitoring mode.The determination was performed on a BEH C18 column (2.1 mm ×100 mm, 1.7 μm) with the mobile phase consisting of acetonitrile-0.1% formic acid with gradient elution at the flow rate of 0.30 mL·min-1. The results showed that the linearities of the 17 analytes had the correlation coefficient and the correlation coefficient were more than 0.99. The limits of quantification were 5 ng/ml and 10 ng/ml for the 17 analytes(10 ng/ml and 25 ng/ml for Olaquindox). The average recoveries and relative standard deviations were 73.87%～116.43% and 1.25～8.44% respectively at 3 spiked levels(10, 25 and 50 ng/mL)(25, 50 and 100 ng/mL for Olaquindox).The proposed method is sensitive, accurate, and efficient. It is applicable for rapid screening and quantification of 17 veterinary drug residues in Maxingshigan oral liquid.