同位素稀释-气相色谱-质谱法测定河蚌蚌肉中邻苯二甲酸酯类残留量

Determination of phthalate acid ester residues in the meat of freshwater mussel by gas chromatography-mass spectrometry

河蚌蚌肉样品采用乙酸乙酯溶剂提取,滤液经弗罗里硅土固相萃取柱净化后氮吹浓缩,正己烷定容,经气质联用仪进行检测,同位素内标法定量。实验结果表明:PAEs在0.10~2.00 mg/L之间具有良好的线性关系,相关系数r^2均大于0.99,对样品进行高、中、低三个浓度的加标试验,各组分的平均回收率在73.1%~94.3%之间,相对标准偏差(RSD)值小于9.3%,检出限在1.2~3.9μg/kg之间。该方法前处理简单,灵敏度和准确度高,可满足河蚌蚌肉中邻苯二甲酸酯类化合物的残留量检测要求。

The fresiiwater mussel samples were extracted witii etiiyl acetate solvent. Tpurified by solid - phase extraction with Florisil column. After filtration, the filtrate was concentrated witi ni-trogen and concentrated with n - hexane. The content was determined by gas chromatography - mass spec-trometry （GC - MS） with isotope internal standard method. The results showed that： PAEs had a good line-ar relationship between 0. 10 -2. 00 mg/L, while the correlation coefficient r2 were all above 0. 99. The aver-age recoveries ranged from 73. 1% to 94. 3% witi RSD that less than 9. 3 % by three level of spiked concen-trations. The limit of detection were ranged from 1. 2 to 3. 9 μg / kg. The method had the advantages of simple pretreatment,high sensitivity and high accuracy, and could be satisfied in requirement of detecting phthalate residues in freshwater mussel meat.