摘要
为提高超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)测定食用植物油中乙基麦芽酚的检测效率,研究其基质效应以评估基质配制标准曲线的必要性,并采取有效的补偿措施。采集市场上常见的各种食用植物油,用甲醇提取,经UPLC-MS/MS检测。采用提取后基质匹配添加法对其基质效应开展全面系统评价。通过稀释样品开展基质效应补偿。结果表明,乙基麦芽酚在2.5~500μg/L范围内线性关系良好,相关系数(R2)为0.999 3。方法的检出限和定量限分别为5.0μg/kg和20μg/kg。在5.0,20和50μg/kg这3个加标水平下的平均回收率为82.7%~95.1%,相对标准偏差不超过7.93%(n=6)。42个样品中34个呈现弱基质效应,为-19.5%~-1.8%,其余8个表现出中等的基质效应,为-20.4%~-39.2%。样品的基质效应随着其色泽的加深而增强。对样品进行适当的稀释可有效降低基质效应。稀释因子为5时,样品的基质效应从中等强度降低至较弱。因此对呈色较浅(淡黄色至黄色)的样品建议直接用溶剂配制工作曲线(2.5~500μg/L)进行定量,而对呈色较深(橙黄色至棕褐色)的样品可进行适当的稀释后采用溶剂配制工作曲线进行定量。
In order to improve detection efficiency of ethyl maltol in edible vegetable oil by ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS),the matrix effects were studied to evaluate the necessity of matrix-matched standard curve,and the effective compensation measures were taken.Various edible vegetable oils commonly found in the market were collected,extracted with methanol and determined by UPLC-MS/MS.Using matrix-matched standard curve,the matrix effects in these samples were assessed comprehensively.Matrix effect compensation was carried out by diluting the sample.The results showed that the linear relationship of ethyl maltol was good in the range of 2.5-500 μg/L,and the correlation coefficient(R2) was 0.999 3.The limits of detection and limit of quantitation were 5.0 μg/kg and 20 μg/kg,respectively.At 3 spiked levels of 5.0,20 and 50 μg/kg,the average recoveries were 82.7%-95.1%,with the relative standard deviations not more than 7.93%(n=6).Matrix effects in 34 out of 42 samples were weak,ranging from-19.5% to-1.8%.The rest were medium,ranging from-20.4% to-39.2%.Matrix effects were enhanced with the deepening of their colors.Matrix effects were reduced effectively by the sample dilution method.When the dilution factor was 5,matrix effects could be ignored.Therefore,for light-colored samples(from light yellow to yellow),preparing solvent standard curve(2.5-500 μg/L)is suggested.For the samples with darker color(form orange yellow to tan),appropriate dilution was necessary.
作者
傅群
刘凤鸣
何毓文
余建兵
FU Qun;LIU Fengming;HE Yuwen;YU Jianbing(Ji'an Food and Drug Inspection and Testing Center,Ji'an 343000)
出处
《食品工业》
CAS
2024年第3期297-301,共5页
The Food Industry
基金
吉安市指导性科技计划项目(20233-0436443)。
关键词
乙基麦芽酚
食用植物油
基质效应
超高效液相色谱-串联质谱法
ethyl maltol
edible vegetable oil
matric effects
ultra-performance liquid chromatography-tandem mass spectrometry
