QuEChERS/UPLC-MS/MS法同时测定梅花鹿鹿茸中36种兽药残留

采用QuEChERS前处理技术,建立了UPLC-MS/MS法同时测定梅花鹿鹿茸中36种兽药残留。鹿茸样品以乙腈-乙酸乙酯(8∶2,V/V)为提取剂,以150 mg乙二胺基-N-丙基、100 mg C18与70 mg中性氧化铝为净化剂。采用Acquity BEH C18色谱柱(2.1 mm×100 mm×1.7μm)分离,25 mmol/L甲酸乙腈溶液和12.5 mmol/L甲酸水溶液为流动相进行梯度洗脱,电喷雾正离子多反应监测模式检测。结果表明:36种兽药在0.1～50μg/L范围内的线性关系良好,相关系数R²均大于0.993,检出限(LOD)为0.08～1μg/kg,定量限(LOQ)为0.3～3μg/kg。向空白样中分别添加浓度为2、5、10μg/kg的36种兽药,平均加样回收率为77.8%～107.6%,相对标准差(RSD)均小于10%。该方法具有操作简便、净化效果显著、灵敏度高、准确性好、检出限低等优点,可用于梅花鹿鹿茸中36种兽药残留的检测。

Determination of 36 Veterinary Drug Residues in Antler Velvet of Cervus nippon Temminck by QuEChERS/UPLC-MS/MS

A method for the simultaneous determination of 36 kinds of veterinary drugs in antler velvet of cervus by UPLC-MS/MS was developed by using the pretreatment technology of dispersed solid phase extraction. Antler samples were extracted with acetonitrile and purified with 150 mg PSA, 100 mg C18 and 70 mg neutral alumina. The target analytes were separated by Acquity BEH C18 column (2.1 mm×100 mm×1.7 μm) with the gradient elution using 25 mmol/L formic acid acetonitrile and 12.5 mmol/L formic acid water as mobile phases. The analytes were detected by positive electrospray ionization with multiple reaction monitoring. The content of 36 kinds of veterinary drugs in pilose antler was quantified by external standard method. The linear relationship of 36 veterinary drugs was good in the range of 0.1-50 μg/L, the correlation coefficients were all greater than 0.993, the LOD was 0.08-1 μg/kg, and the LOQ was 0.3-3 μg/kg. 36 kinds of veterinary drugs with concentrations of 2, 5, 10 μg/kg were added to the blank sample. The average recovery was 77.8%-107.6%, and the relative standard deviation was less than 10%. The method has the advantages of simple operation, remarkable purification effect, high sensitivity, good accuracy and low detection limit, which can be used for the determination of 36 kinds of veterinary drugs in antler velvet of Cervus nippon Temminck.