高效液相色谱-串联四极杆质谱结合液液萃取净化测定乳制品中莫奈太尔砜残留量

Determination of monepantel sulfone residue in dairy products by high performance liquid chromatography tandem mass spectrometry combined with liquid-liquid extraction purification

中文关键词:  莫奈太尔砜  高效液相色谱-串联质谱法  乳制品  残留

英文关键词:monepantel sulfone  high performance liquid chromatography-tandem mass spectrometry  dairy products  residue

中文摘要:

      目的 建立高效液相色谱-串联质谱法(high performance liquid chromatography tandem mass spectrometry, HPLC-MS/MS)测定乳制品中莫奈太尔砜残留的检测方法。方法 样品经水-饱和氯化钠-乙腈溶液提取, 正己烷净化。用Inertsil C8-3(100 mm×2.1 mm, 3 μm)分离, 以甲醇和水溶液为流动相进行梯度洗脱, 质谱采用多离子检测模式(multi reaction monitor, MRM)对莫奈太尔砜的定量离子和定性离子进行监测, 外标法定量。结果 莫奈太尔砜在0.1~5.0 μg/L质量浓度范围内线性关系良好。莫奈太尔砜在2.0、4.0和20 μg/kg浓度的回收率为85.0%~102.9%, 相对标准偏差小于4.9% (n=6), 定量限为2.0 μg/kg。结论 该方法快速、准确、灵敏, 适合测定乳制品中莫奈太尔砜药物残留量。

英文摘要:

      Objective To establish a method for determination of monepantel sulfone in dairy products by high performance liquid chromatography-tandem mass spectrometry (HPLC–MS/MS). Methods Samples were extracted with water, saturated sodium chloride solution and acetonitrile. The extracts were purified by hexane, and then the monepantel sulfone residue in the extracts were separated by Inertsil C8-3 (100 mm×2.1 mm, 3 μm) with methanol and water as mobile phase for gradient elution. Using HPLC–MS/MS with multiple reactions monitoring (MRM), identification of the major components of the monepantel sulfone residue was performed based upon the intensities of fragments. The quantification was performed by the external standard method. Results The calibration curves showed good linearities in the range of 0.1~5.0 μg/L. The recoveries were ranged from 85.0% to 102.9% for the monepantel sulfone residues with 3 spiked levels of 2.0, 4.0 and 20 μg/kg. The relative standard deviations (RSDs) were less than 4.9% (n=6), and the limit of quantitation (LOQ) for the monepantel sulfone was 2.0 μg/kg. Conclusion The proposed method is rapid, accurate and sensitive, which is suitable for detecting monepantel sulfone residue in dairy products.