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  

Determination of Chlormequat Residues in Grains and Oils by Gas Chromatography-Tandem Massspectrometry with QuEChERS

作　　者：刘付英 杨水艳 郭颖 邵志凌 LIU Fu-ying;YANG Shui-yan;GUO Ying;SHAO Zi-lin(Yunnan Grain and Oil Science Research Institute(Yunnan Grain and Oil Product Quality Supervision and Inspection Center),Kunming,Yunnan 650033,China)

机构地区：[1]云南省粮油科学研究院(云南省粮油产品质量监督检验测试中心),云南昆明650033

出　　处：《粮油食品科技》2022年第5期234-243,共10页Science and Technology of Cereals,Oils and Foods

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-GCMS/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0.05~2μg/mL浓度范围内有较好的线性关系,相关系数R2均大于0.9980。检出限为0.004~0.009 mg/kg,定量限为0.01~0.03mg/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。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(C)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 0.05~2μg/m L for CCC in different matrixes,with correlation coefficients(R~2)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.

关 键 词：气相色谱串联质谱法 粮谷 油料油脂 矮壮素 

分 类 号：TS210.7[轻工技术与工程—粮食、油脂及植物蛋白工程]