建立了 LPAS(Lipid and protein adsorbent)快速滤过型净化柱结合气相色谱-串联质谱测定油料中60种持久性有机污染物(Persistent organic pollutants,POPs)残留量的方法.样品经乙酸乙酯超声提取,提取液在-18 ℃冷冻2 h后经LPAS快速滤过型净化柱净化,用气相色谱-串联质谱在多反应监测模式下检测.结果表明:60种POPs在0.5～100 μg/L范围内线性良好,相关系数均大于0.9951,检出限为0.2～3.0μg/kg,定量限为0.5～8.0 μg/kg;在大豆和花生2种基质中,加标水平为0.5～80.0 μg/kg时,回收率为66.2％～118.3％,相对标准偏差为0.8％～9.9％.利用该方法检测市售30例样品,阳性检出率为6.6％.该检测方法操作简单,定性定量准确,适用于油料中POPs残留的快速筛查.
Determination of 60 Persistent Organic Pollutants Residues in Oil Crops by Gas Chromatography-Tandem Mass Spectrometry Based on Rapid Filtration Cleanup
A method for determination of residues of 60 persistent organic pollutants(POPs)in oil crops was established by lipid and protein adsorbent(LPAS)rapid filtration cleanup column combined with gas chromatography-tandem mass spectrometry(GC-MS/MS).The samples were ultrasonically extracted with ethyl acetate,and the extracts were frozen at-18℃ for 2 h,then purified with the LPAS rapid filtration cleanup,the analytes were detected by GC-MS/MS at multiple reaction monitoring mode.The results showed the linear relationships for 60 POPs were good in the range of 0.5-100 μg/L,and the correlation coefficients were above 0.9950.The limits of detection were in the range of 0.2-3.0 μg/kg and the limits of quantitation were in the range of 0.5-8.0 μg/kg.For soybean and peanut matrices,at spiked levels of 0.5 μg/kg to 80 μg/kg,the average recoveries were in range of 66.2％-118.3％and relative standard deviations were in range of 0.8％-9.9％.30 samples were detected by the method,and the detection rate of positive samples was 6.6％.This detection method is simple to operate,accurate for qualitative and quantitative analysis,and suitable for the rapid screening of POPs residues in oil crops.
LPAS rapid filtration cleanupgas chromatography-tandem mass spectrometrypersistent organic pollutantsoil crops
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