超高效液相色谱-串联质谱法检测猪肌肉组织中烯丙孕素残留

Determination of altrenogest in pork muscle tissue by ultra-high performance liquid chromatography-tandem mass spectrometry

建立了测定猪肌肉组织中烯丙孕素残留的超高效液相色谱-串联质谱方法。试样经乙腈和乙酸乙酯提取,低温冷冻去除脂类。采用C18反相色谱柱进行分离,以乙腈-0.1%甲酸水为流动相梯度洗脱,电喷雾离子源正离子模式下多反应监测模式检测,基质匹配外标法定量。结果表明,烯丙孕素在1~50ng/mL浓度范围内线性良好,相关系数大于0.99;该方法在猪肌肉组织中检测限(S/N=3)和定量限(S/N=10)分别为0.3μg/kg和1.0μg/kg。加标回收率68.5%~87.9%,日内变异系数1.1%~6.0%,日间变异系数5.5%~10.7%。方法快速、准确、灵敏度高,能满足猪肌肉组织中烯丙孕素残留定性定量分析。

The samples were extracted with acetonitrile and ethyl acetate,and the lipids was removed by cryogenic freeze. C^8 reversed phase chromatographic column was used as the separation column and acetonitrile-0. 1 % formic acid water was used as the mobile phase. The scanning was monitored at multi- response monitoring mode （MRM） and the positive ions electrospray ion source mode was applied simultaneously, using the matrix matching external standard method for quantitative analysis. The results showed that altrenogest was linear in the corresponding concentration range of 1-50 ng/mL, and the correlation coefficient was larger than 0.99. The detection limit （LOD, S/N= 3） and quantitative limit （LOQ, S/N = 10） of this method were 0.3 μg/kg and 1.0 μg/kg, respectively. At the level of 3 spiked concentrations, the recoveries ranged from 68.5% to 87.9%, the variation coefficient of the intra-batch was within 1.1%-6.0%, and the coefficient variation of the inter-batch was within 5.5 %-10. 7%. The method is rapid, precise, and suitable for qualitative and quantitative analysis of altrenogest in pork muscle tissue.