高效液相色谱-串联质谱法测定食用槟榔中4种黄曲霉毒素的含量

HPLC-MS/MS Determination of 4 Aflatoxins in Edible Areca-Nut

将粉碎后的槟榔样品2.00g用20mL乙腈提取,以100mg N-丙基乙二胺为净化剂分散固相萃取净化萃取液。取上清液以Thermo Accucore aQ C18色谱柱为固定相,以0.005mol·L-1乙酸铵溶液-乙腈混合液为流动相进行梯度洗脱,采用高效液相色谱-串联质谱法测定其中4种黄曲霉毒素的含量。质谱分析中采用电喷雾离子源和多反应监测模式。结果表明:4种黄曲霉毒素的质量浓度均在0.1～10.0μg·L-1内与其峰面积呈线性关系,测定下限(10S/N)为1μg·kg-1。以食用槟榔样品为基质,按标准加入法进行回收试验,回收率为80.0%～99.2%,测定值的相对标准偏差(n=6)为1.5%～9.3%。

The crushed areca-nut sample of 2.00 g was extracted with acetonitrile of 20 mL, and the extracte was cleaned up by dispersive solid phase extraction with 100 mg of N-propylethylenediamine as purificant. Thermo Accucore aQ C18 column was used as stationary phase, and the mixture of 0.005 mol · L^-1 ammonium acetate solution and acetonitrile was used as mobile phase for gradient elution. Four aflatoxins in the supernatant were determined by high performance liquid chromatography-tandem mass spectrometry （HPLC-MS/MS）. The electrospray ion source and the multi reaction monitoring mode were adopted in MS analysis. As shown by the results, linear relationships between values of peak area and mass concentration of the 4 aflatoxins were found in the same range of 0.1-10.0 μg · L^-1 , with lower limits of determination （10S/N） of 1 μg · kg^-1. Test for recovery by standard addition method was made on the base of edible areca-nut sample, giving results in the range of 80.0%- 99.2%, and RSDs （n=6） ranged from 1.5% to 9.3%.