固相萃取-高效液相色谱-串联质谱法同时测定羊肉中3种β-兴奋剂

Simultaneous Determination of Three β-agonists in Mutton by Solid Phase Extraction Coupled with High Performance Liquid Chromatography-Tandem Mass Spectrometry

利用固相萃取-高效液相色谱-串联质谱技术,建立了羊肉中克伦特罗、莱克多巴胺、沙丁胺醇3种β-兴奋剂的测定方法。样品经乙酸铵缓冲溶液提取后,用MCX固相萃取柱净化,以甲酸-乙腈和甲酸-乙酸铵缓冲溶液为流动相,梯度洗脱,采用HPLC-MS/MS电喷雾正离子(ESI+)电离,多反应监测(MRM)模式检测,外标法定量。结果表明,3种β-兴奋剂在2-100 ng/mL范围内均具有良好的线性关系,相关系数不低于0.998 8,加标回收率为91.3%～103.8%,相对标准偏差为2.5%-5.7%。该方法准确、灵敏、高效、环保,适用于羊肉中克伦特罗、莱克多巴胺、沙丁胺醇3种β-兴奋剂的同时测定。

A soild phase extraction-high performance liquid chromatography-tandem mass spectrophy （HPLC-MS/MS）was developed for determination of three β-agonists such as clenbuterol, ractomine, salbutemol residues in mutton. The samples were extracted by ammonium acetate buffer, and purified by MCX solid-phase extraction column. Using Formic aeid-acetonitrile and formic acid-ammonium acetate buffer as mobile phase by gradient elution, the analysis of target compounds was carried out by HPLC-MS/MS under positive electrospray ionization （ESI^＋） and multiple reaction monitoring （MRM）mode. An external standard was employed for quantitative analysis. The calibration curves were in good linearity between the peak area and the concentration of 2 to 100 ng/mL for three β-agonists with correlation coefficients not less than 0.998 8. The spiked recoveries ranged from 91.3% to 103.8% with relative standard deviations of 2.5% to 5.7%. The proposed method is accurate, sensitive and high-efficient ,and is applicable for simultaneous determination of three β-agonists in mutton.