蔬菜基质对气质法测定有机磷和聚酯类农药残留的影响  

The Influence of Vegetable Substrate on the Determination of Organic Phosphorus and Polyester Pesticide Residues by Gas Chromatography-mass Spectrometry

作　　者：刘兰 刘培勇 张良成 张惠 符丹 王毅 LIU Lan;LIU Peiyong;ZHANG Liangcheng;ZHANG Hui;FU Dan;WANG Yi(Dazhou Food and Drug Inspection Institute,635000)

机构地区：[1]达州市食品药品检验所,达州635000

出　　处：《食品工业》2024年第3期310-313,共4页The Food Industry

摘　　要：验证萝卜、上海青、生姜3种基质标准工作液以及色谱柱分离条件对测定毒死蜱、高效氯氟氰菊酯2类农药残留测定结果的准确性影响。研究萝卜、上海青、生姜空白基质配制成3种基质的工作标准溶液和调整气相色谱柱分析条件,测定3种蔬菜样品的加标回收率及基质标准工作液交叉相互测定。结果表明:方法最低检出限为0.000 88 mg/kg,萝卜基质毒死蜱线性范围为0.005~0.5μg/mL,r~2=0.999 899 69;萝卜基质高效氯氟氰菊酯线性范围为0.005~0.5μg/mL,r~2=0.999 821 41。生姜基质毒死蜱线性范围为0.005~0.5μg/mL,r~2=0.999 927 79;生姜基质高效氯氟氰菊酯线性范围为0.005~0.5μg/mL,r~2=0.999 902 86。上海青基质毒死蜱线性范围为0.005~0.5μg/mL,r~2=0.999 800 60;上海青基质高效氯氟氰菊酯线性范围为0.005~0.5μg/mL,r~2=0.999 640 33。毒死蜱加标量为0.5 mg/kg、高效氯氟氰菊酯加标量为0.4 mg/kg,n=6。3种空白基质标液对萝卜、小白菜、仔姜的测定精密度显示:小白菜加标毒死蜱SRSD为4.6%,高效氯氟氰菊酯SRSD为8.5%;萝卜加标毒死蜱SRSD为5.5%,高效氯氟氰菊酯SRSD为5.9%;仔姜加标毒死蜱SRSD为6.5%,高效氯氟氰菊酯SRSD为5.5%。精密度均小于10%。加标回收率均在86.2%~105.2%之间。基质标准溶液互测3种样品加标结果重现性好,精密度高。采用该方法任意选择3种蔬菜中的一种作为空白基质配制标准工作液测定毒死蜱、高效氯氟氰菊酯,都具有准确性高、重现性好的特点,对蔬菜农药分析工作具有深远意义。Verify the accuracy of determining chlorpyrifos and beta-cyhalothrin residues in radish,Shanghai Green and ginger by standard working solution and chromatographic column.The standard working solutions of Radish,Shanghai Green and ginger are prepared,and the recoveries of the three vegetable samples are determined by adjusting the conditions of gas chromatography.The results show that the recoveries of radish,Chinese cabbage and ginger are in the range of 86.2% to 105.2%.The minimum detection limit is 0.000 88 mg/kg,and the linear range of phorate in radish matrix is 0.005-0.5 μg/mL,with r~2=0.999 899 69.The linear range of cyhalothrin in radish matrix is 0.005-0.5 μg/mL,with r~2=0.999 821 41.The linear range of phorate in ginger matrix is 0.005-0.5 μg/mL,with r~2=0.999 927 79.The linear range of cyhalothrin in ginger matrix is 0.005-0.5 μg/mL,with r~2=0.999 902 86.The linear range of phorate in Shanghai green(bok choy) matrix is 0.005-0.5 μg/m L,with r~2=0.999 800 60;The linear range of cyhalothrin in Shanghai green matrix is 0.005-0.5 μg/mL,with r~2=0.999 640 33.The spiked level of phorate is 0.5 mg/kg,and that of cyhalothrin is 0.4 mg/kg,with n=6.The results of three kinds of samples of matrix standard liquid are good in repeatability and high in precision.The method is accurate and reproducible for the determination of chlorpyrifos and cyhalothrin in one of the three kinds of vegetables,and it has far-reaching significance to the analysis of vegetable pesticide.

关 键 词：气质法 基质 影响 

分 类 号：O657.63[理学—分析化学] TS255.7[理学—化学]