HPLC-MS法同时测定羊肉中14种β-受体激动剂残留

Simultaneous Determination of 14β-Agonists Residues in Mutton by HPLC-MS/MS

建立高效液相色谱-串联质谱法(HPLC-MS/MS)测定羊肉中14种β-受体激动剂残留量的分析方法。样品经β-葡萄糖醛苷酶水解后,经5%乙酸-乙腈(1∶99,V/V)溶液提取,利用三种吸附剂(无水硫酸镁、C18粉和N-丙基乙二胺)净化洗脱,选用Eclipse plus C_(18)色谱柱分离,采用多反应监测(MRM)模式定性,基质标准溶液外标法定量。在优化条件下,14种β-受体激动剂的保留时间在1.0~9.5 min之间。当质量浓度范围在0.05~0.5μg/mL时,各种β-受体激动剂的线性关系良好,相关系数(r)均≥0.9992,方法检出限(LOD,r_(SN)=3)为0.04μg/kg~0.87μg/kg,定量限(LOQ)0.35μg/kg~1.86μg/kg,在5.0,50和100μg/kg浓度水平上加标平均回收率为82.8%~108.9%,相对标准偏差(n=6)为1.9%~6.7%。该方法操作简单、准确,可快速定性定量分析羊肉中14种β-受体激动剂的残留。

To establish a method for the simultaneous detection of 14β-agonists residues in mutton by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS),the samples were added to ammonium acetate buffer and enzymatic hydrolysis byβ-Glucuronidase.The hydrolyzates extracted with acetonitrile containing 5%acetic acid(1∶99,V/V),and then the extract was cleaned up by the powder of magnesium sulfate,C_(18) and primary secondary amine(PSA).The target analytes were separated on an Eclipse plus C18 column,determined using electrospray ionization(ESI)source in positive mode with the multiple reaction monitoring(MRM)acquisition mode and quantifed with the matrix-matched external standard method.Retention time for the 14β-agonists were found in the range from 1.0 min to 9.5 min under the optimized conditions.The linear relation was good when the concentration range was of 0.05μg/mL to 0.5μg/mL,the correlation coefficient of the 14β-agonists were≥0.9992,the limits of detection were in the range of 0.04μg/kg to 0.87μg/kg,the limits of quantifcation were in the range of 0.35μg/kg to 1.86μg/kg,the average recoveries in the sample additive experiment at 3 concentration levels was 82.8%-108.9%,and the relative standard deviations were in the range of 1.9%-6.7%.The proposed procedure was simple,quick and accurate for the simultaneous determination of the 14β-agonists in mutton.