QuEChERS结合GC-MS/MS测定酱腌菜中11种N-亚硝胺类化合物
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仙居县食品药品检验检测中心,浙江 台州 317300

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管悦 女 主管药师 研究方向为食品药品检测 E-mail:13023216213@126.com

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R155

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Determination of 11 N-nitrosamines in Chinese pickles and salted vegetables by QuEChERS combined with GC-MS/MS
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Xianju County Food and Drug Inspection and Testing Center, Zhejiang Taizhou 317300, China

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    摘要:

    目的 建立QuEChERS结合气相色谱-质谱联用法同时测定酱腌菜中11种亚硝胺类化合物含量的高效分析方法。方法 样品使用乙腈提取,经4 g无水硫酸镁和1 g氯化钠脱水,150 mg PSA、150 mg GCB和900 mg无水硫酸镁净化,采用HP-Innowax色谱柱分离,多反应监测模式下定量分析,并通过计算基质与溶剂标准曲线间斜率的比值来评估基质效应。结果 11种N-亚硝胺类化合物在0.5~50 μg/L线性范围内,线性决定系数均>0.999,NDBA、NMPhA、NEPhA、NDPhA呈较强的基质效应,应采用空白基质配标法,低、中、高三个水平(1、3、10 μg/kg)加标试验的平均回收率为94.8%~105.1%,RSD(n=6)为1.6%~5.8% 。结论 该方法前处理操作简单、重复性好、结果准确,适用于酱腌菜中11种N-亚硝胺类化合物的定量分析。

    Abstract:

    Objective To establish an efficient analytical method for simultaneous determination of 11 N-nitrosamines in Chinese pickles and salted vegetables by QuEChERS combined with gas chromatography-mass spectrometry.Methods The sample was extracted with acetonitrile, dehydrated by 4 g anhydrous magnesium sulfate and 1 g sodium chloride, purified with 150 mg PSA, 150 mg GCB and 900 mg anhydrous magnesium sulfate, separated by HP-Innowax chromatographic column, and quantitatively analyzed in the multi-reaction monitoring mode. The matrix effect was evaluated by calculating the ratio of the slope between the matrix and the solvent standard curve.Results In the range of 0.5-50 μg/L, the linear coefficient of 11 N-nitrosamines were all above 0.999. NDBA, NMPhA, NEPhA and NDPhA showed stronger matrix effects, and the standard solution should be prepared by the blank matrix solution. The average recovery rate of low, medium and high levels (1, 3, 10 μg/kg) in the sample spiking with reference standard was 94.8%-105.1%, of which the RSD (n=6) was 1.6%-5.8%.Conclusion With simple pretreatment operation, good reproducibility and accurate results, this method is suitable for the quantitative analysis of 11 N-nitrosamines in Chinese pickles and salted vegetables.

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管悦,泮燕媚. QuEChERS结合GC-MS/MS测定酱腌菜中11种N-亚硝胺类化合物[J].中国食品卫生杂志,2022,34(6):1226-1232.

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  • 收稿日期:2021-05-12
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  • 在线发布日期: 2023-02-06
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