摘要:
采用分散固相萃取的前处理技术,建立了一种UPLC-MS/MS(ultra performance liquid chromatography-tandem mass spectrometry)法同时测定梅花鹿鹿茸中7种镇静剂的检测方法。鹿茸样品以2%氨水乙酸乙酯为提取剂,200 mg C18为净化剂。液相色谱条件:ACQUITY BEH C18柱(2.1 mm×100 mm,1.7 μm),流动相A为0.1%甲酸乙腈,B为水,柱温35 ℃;质谱条件:正离子模式(ESI+),多反应监测(multiple reaction monitoring,MRM)模式,鹿茸中镇静剂含量采用外标法定量。结果表明,7种镇静剂在0.3~100 ng/mL内线性关系良好,决定系数R2均大于0.992,7种镇静剂的LOD(limits of detection)为0.3 μg/kg,LOQ(limit of quantitation)为1 μg/kg,平均加样回收率为82.6%~107.3%,相对标准偏差RSD(relative standard deviation)均小于5%。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7种镇静剂的检测。
Abstract:
A method for the simultaneous determination of 7 sedatives in antler velvet of Cervus nippon Temminck by UPLC-MS/MS was developed by using pre-treatment technology of dispersive solid phase extraction. The antler velvet sample was treated with 2% aqueous ammonia ethyl acetate as an extractant and 200 mg C18 as a purifying agent. Liquid chromatography conditions:ACQUITY BEH C18 column(2.1 mm×100 mm,1.7 μm),mobile phase A was 0.1% formic acid acetonitrile,B was water,column temperature was 35 ℃. Mass spectrometry conditions:Positive ion mode(ESI+),multiple reactions monitoring mode. The sedative contents in antler velvet were quantified by external standard method. The linearity of the 7 sedatives in 0.3~100 ng/mL was good,the correlation coefficient R2 was greater than 0.992,and the LOD of the 7 sedatives was 0.3 μg/kg,LOQ was 1 μg/kg,the average recovery rate was 82.6%~107.3%,and the RSD was less than 5%. The method had the advantages of simple operation,remarkable purification effect,high sensitivity,good accuracy and low detection limit. It could be used for the determination of 7 sedatives in antler velvet of Cervus nippon Temminck.
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