QuEChERS结合GC-MS/MS检测大米中六六六和滴滴涕残留量的方法建立
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1.河南省食品和盐业检验技术研究院(河南省粮油饲料产品质量监督检验中心),河南 郑州 450000;2.国家市场监管重点实验室(食品安全快速检测与智慧监管技术),河南 郑州 450003

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彭星星(1989—),女,硕士,工程师,主要从事粮油食品检验研究。E-mail:568464200@qq.com

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河南省市场监督管理局2024年度科技计划项目(HNSCJGK202491)。


Determination of Residues of Hexachlorocyclohexanes and Dichlorodiphenyltrichloroethanes in Rice by QuEChERS Combined with GC-MS/MS
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1.Henan Institute of Food and Salt Industry Inspection Technology (Quality Supervision and Inspection Center of Grain, Oil and Feed Product in Henan Province), Zhengzhou 450000, China;2.Key Laboratory of Food Safety Quick Testing and Smart Supervision Technology for State Market Regulation, Zhengzhou 450003, China

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    摘要:

    目的】建立一种QuEChERS结合气相色谱-质谱联用(GC-MS/MS)的检测方法,用于检测大米中六六六和滴滴涕的残留量。【方法】大米样品加水混匀,经乙腈醋酸溶液提取、PSA和C18固相萃取净化、氮吹浓缩定容后,使用GC-MS/MS测定,内标法定量。【结果】4种六六六和4种滴滴涕在质量浓度为6.25~100.00 ng/mL时线性关系较好,相关系数(R2)均大于0.999,检出限为0.000 2~0.000 5 mg/kg,定量限为0.000 5~0.002 0 mg/kg;基质加标回收率为92.27%~98.76%,相对标准偏差(RSD)为0.44%~1.88%;质控样品测试值均在真值范围内,考核样品的比对结果均为满意。【结论】该方法灵敏度高,重复性和准确性好,适用于大米中六六六和滴滴涕残留量的快速测定。

    Abstract:

    [Objective] To establish a method for the quantitative detection of residues of hexachlorocyclohexanes (BHCs) and dichlorodiphenyltrichloroethanes (DDTs) in rice by combining QuEChERS with gas chromatography-tandem mass spectrometry (GC-MS/MS). [Method] Rice samples were mixed with water and extracted with acetonitrile-acetic acid solution. The extracts were purified by PSA/C18 solid phase extraction. After high-speed centrifugation and concentration by nitrogen flushing, the samples were detected by GC-MS/MS, and the internal standard method was used for quantitation. [Result] Four BHCs and four DDTs showed excellent linearity within the mass concentration range of 6.25~100.00 ng/mL, with R2 greater than 0.999. The limits of detection and quantitation were within the ranges of 0.000 2~0.000 5 mg/kg and 0.000 5~0.002 0 mg/kg, respectively. The average recovery rates of matrix addition were between 92.27% and 98.76%, and the relative standard deviations (RSD) were between 0.44% and 1.88%. Quality control samples for validation were detected by the established method, and the results were within the true value range. The comparison results of the samples participating in the assessment were all satisfactory. [Conclusion] The established method demonstrates high sensitivity, good repeatability, and high accuracy, being suitable for rapid determination of residues of BHCs and DDTs in rice.

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彭星星,高海军. QuEChERS结合GC-MS/MS检测大米中六六六和滴滴涕残留量的方法建立[J].食品与生物技术学报,2025,(1):165-172.

PENG Xingxing, GAO Haijun. Determination of Residues of Hexachlorocyclohexanes and Dichlorodiphenyltrichloroethanes in Rice by QuEChERS Combined with GC-MS/MS[J]. Journal of Food Science and Biotechnology,2025,(1):165-172.

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  • 收稿日期:2023-09-18
  • 最后修改日期:2023-11-17
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  • 在线发布日期: 2025-05-12
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