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QuEChERS-气相色谱–串联质谱法测定粮谷和油料油脂中矮壮素残留
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Determination of Chlormequat Residues in Grains and Oils by Gas Chromatography-Tandem Massspectrometry with QuEChERS
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    摘要:

    通过前处理及仪器条件优化,建立了QuEChERS-气相色谱-串联质谱法(QuEChERS-GC- MS/MS)法测定粮食和油料油脂中矮壮素残留的分析方法。选用小麦粉、大米、玉米、大豆、大豆油、油菜籽、菜籽油作为样品,样品经乙腈提取,无水硫酸镁和氯化钠盐析脱水、再经N-丙基乙二胺(PSA)、十八烷基键合硅胶(C18)吸附剂净化。采用衍生质谱方法考察了不同基质(小麦粉、大米、油菜籽、菜籽油)的基质效应,基质匹配外标法定量。结果表明,不同基质中矮壮素在0.05~2 μg/mL浓度范围内有较好的线性关系,相关系数R2均大于0.998 0。检出限为0.004~0.009 mg/kg,定量限为0.01~0.03 mg/kg;在3个添加水平下的平均加标回收率为73.6%~99.1%,相对标准偏差(RSD)为2.34%~7.78%(n=6)。该方法高效、灵敏度高,可满足粮谷和油料油脂样品中矮壮素残留量的检测要求。

    Abstract:

    The aim of this study is to develop a method for the determination of chlormequat (CCC) residues in grain and oil. The pretreatment by using QuEChERS and Gas Chromatography-Tandem Massspectrometry (GC-MS/MS) analysis were optimized. The samples were extracted from wheat flour, rice, corn, soybean, soybean oil, rapeseed, and rapeseed oil with acetonitrile and salted out with anhydrous magnesium sulfate, and sodium chloride, then cleaned up by a mixture of N-propyl ethylenediamine (PSA) and octadecyl silane (C18) adsorbents. The matrix effects of different substrates (wheat flour, rice, rapeseed, rapeseed oil) were investigated by derived mass spectrometry and matrix-matched calibration combined with external standards was used for quantitative analysis. The results showed a good linearity in the range of 0.05~2 μg/mL for CCC in different matrixes, with correlation coefficients (R2) of more than 0.9980. The limits of detection (LODs) and the limits of quantification (LOQs) of the method were 0.004~0.009 mg/kg and 0.01~0.03 mg/kg, respectively. The averagerecoveries at three spiked levels were 73.6%~99.1%, and the relative standard deviations (RSDs) were 2.34%~7.78% (n = 6). The method was efficient and sensitive, and satisfied the testing requirements for chlormequat residues in grain and oil samples.

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刘付英,杨水艳*,郭 颖,邵志凌. QuEChERS-气相色谱–串联质谱法测定粮谷和油料油脂中矮壮素残留[J].粮油食品科技,2022,30(5):234-243.

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  • 在线发布日期: 2022-09-26
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