液相色谱-串联质谱法检测猪肉中20种违禁药物残留的研究

Multi-class residue analysis of illicit drugs in pork by high performance liquid chromatography-tandem mass spectrometry

关键词:  高效液相色谱-串联质谱法  违禁药物  残留检测

Key words:  Multi-class Residue Analysis of 20 Illicit Drugs in Pork by High Performance Liquid Chromatography-tandem Mass Spectrometry

摘要:

建立了猪肉中违禁药物（糖皮质激素、性激素、β2-肾上腺素受体激动剂、玉米赤霉烯酮4类）同时测定的高效液相色谱-串联质谱方法。试样经盐酸水解，乙酸乙酯提取，低温冷冻去除脂类，亲水亲脂平衡固相萃取柱净化。采用C18反相色谱柱分离，以乙腈+水为流动相梯度洗脱，分别在电喷雾离子源正、负离子模式下以多反应监测模式（MRM）分段扫描同时检测，基质匹配内标法定量。结果表明，20种违禁药物在相应的浓度范围内线性良好，相关系数均大于0.99；该方法在猪肉中的检测限（LOD，S/N=3）和定量限（LOQ，S/N=10）分别为0.5、1.0 μg/kg。在0.5~10 μg/kg添加浓度水平下，平均回收率为63.9%~117%，批内变异系数1.9%~9.1%，批间变异系数4.9%~13.1%。该方法简单、快速、准确，适用于猪肉中多类违禁药物的残留检测。

Abstract:

A simultaneous multi-class analysis method for illicit drugs (glucocorticoid hormones, sex hormones,β-agonists,zearanlenone) in pork by high performance liquid chromatography-tandem mass spectrometry was established. The samples were hydrolyzed by dilute hydrochloric acid, extracted by ethyl acetate and cryogenically frozen to remove most lipids followed by clean-up with hydrophilic lipophilic balance SPE. The quantification and confirmation of the 20 analytes were performed by LC-MS/MS with electro-spray ionization (ESI) interface in multiple reaction monitoring (MRM) mode. Matrix matching internal standard method was hired for quantitative analysis. The results showed that 20 illicit drugs were linear in the corresponding concentration range, and the correlation coefficient was greater than 0.99. The limits of detection (LODs) and limits of quantification (LOQs) were 0.2~0.5 μg/kg and 0.5~1.0 μg/kg, respectively. The spiked recoveries at three levels were from 63.9% to 117%. The repeatability and the within-laboratory reproducibility were from 1.9% to 9.1% and from 4.9% to 13.1%, respectively. The method is simple, rapid,accurate and suitable for simutaneous residue detection of multi-class illicit drugs in pork.