超高效液相色谱-串联质谱法测定肉制品中的克伦特罗

Determination of clenbuterol in meat products by ultra performance liquid chromatography-tandem mass spectrometry

目的建立超高效液相色谱-串联质谱法测定肉制品中克伦特罗残留量的方法。方法样品采用0.1 mol/L的高氯酸溶解提取、正己烷脱脂,将高氯酸提取液调节至pH=5.0后,采用PXC固相萃取柱(60 mg,3 mL)进行除杂净化。选用乙腈(A)和0.1%(V/V)甲酸水溶液(B)作为流动相,Agilent Eclipse C_(18)(50 mm×2.1 mm,1.8μm)作为分离色谱柱,在电喷雾离子源(ESI)正离子模式下以多反应检测(multiple reaction monitoring,MRM)采集数据并做定性筛查和定量分析。结果克伦特罗在0.1~100μg/L浓度范围内线性关系良好,相关系数大于0.99,检出限(S/N≥3)为0.02μg/L,方法的平均回收率为91.35%~102.42%;相对标准偏差(n=6)为1.14%~4.52%。结论该方法前处理操作简便、样品分离效果好、成本低、回收率和重现性好,适用于肉制品中克伦特罗的测定。

Objective To establish a method for the determination of clenbuterol in meat products by ultra performance liquid chromatography-tandem mass spectrometry. Method The sample was extracted with 0.1 mol/L perchloric acid and degreased with hexane. The perchloric acid extract was adjusted to pH 5.0 and then cleaned up by PXC SPE column （60 mg, 3 mL）. Acetonitrile （A） and 0.1% （V：V） aqueous formic acid （B） were used as the mobile phase, Agilent Eclipse C18 （50 mm×2.1 mm, 1.8 μm） was used as the separation column, and the samples were determined in an electrospray ion source （ESI） positive ion mode of multiple reaction monitoring （MRM） to collect data and make qualitative screening and quantitative analysis. Results In the concentration range of 0.1~100 μg/L, the linear relationship was good with the correlation coefficient greater than 0.99, and the limit of detection （S/N≥3） was 0.02 μg/L. The average recovery of clenbuterol was 91.35%~102.42%, and the relative standard deviations （n=6） were 1.14%~4.52%. Conclusion This method has simple pretreatment process, good separation effect, low cost, good recovery and reproducibility, which is suitable for the determination of clenbuterol in meat products.