气相色谱-串联质谱法快速测定禽蛋中203种农药及化学污染物残留

Simultaneous determination of 203 pesticide and chemical pollutant residues in eggs by gas chromatography-tandem mass spectrometry

建立了禽蛋中203种农药及化学污染物残留的气相色谱一串联质谱（GC—MS／MS）检测方法。样品用乙腈振荡提取，经ODSC，。＋Carb串联固相萃取柱净化，乙腈一甲苯（3：1，v／v）洗脱，洗脱液浓缩至0．5mL，氮吹至近干，加1mL正己烷超声溶解后，在气相色谱．串联质谱多反应监测（MRM）模式下进行测定。在1倍MRL（最大允许残留限量）、3倍MRL和5倍MRL三个添加水平下，鸡蛋、鹌鹑蛋中203种分析物的添加回收率均在60％～120％的有183种，占研究总数的90．1％；相对标准偏差均〈20％的有197种，占研究总数的97．0％。203种分析物中线性范围超过2个数量级的有192种，占94．6％，所有分析物的线性相关系数均〉0．99。方法的检出限为0．03～181．9μg／kg。

A method has been developed for the simuhaneous determination of 203 residues in eggs by gas chromatography-tandem mass spectrometry （GC-MS/MS）. Samples were extracted with acetonitrile, cleaned-up by an ODS Cj8 ＋ Carb solid phase extraction cartridge, the eluate was concentrated to ca 0. 5 mL, nitrogen to near dry, and then 1 mL of hexane was added into the sample and mixed thoroughly by ultrasonic. Finally, the sample solution was determined by GC-MS/MS （MRM）. This method was evaluated at three spiked levels of 1 times, 3 times and 5 times of MRL（Maximum Residue Limits） in 3 parallel experiments for egg and quail egg resPectively. The results showed that the number of pesticides with the recoveries between 60% and 120% is 183, accounted for 90. 1%. The number of pesticides with RSD≤20% was 197, accounted for 97.0%. Linear ranges for 192 pesticides were over 2 orders of magnitude. The correlation coefficients of all the pesticides were over 0.99. The LODs were from 0.03 μg/kg to 181.9 μg/kg. This method is effective, selective, sensitive, accurate and easy to be operated.