首页|改良SinChERS结合电喷雾离子源-三重四级杆质谱测定茶叶中灭螨醌及其代谢物的方法研究

改良SinChERS结合电喷雾离子源-三重四级杆质谱测定茶叶中灭螨醌及其代谢物的方法研究

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文章建立了一种基于SinChERS净化技术结合超高压液相色谱-串联质谱法测定茶叶中灭螨醌及其代谢物羟基灭螨醌残留量的检测方法.样品经1%甲酸乙腈提取,用SinChERS-TPR进行净化,经Agilent C18色谱柱分离,以0.1%甲酸水-甲醇作为流动相进行梯度洗脱,电喷雾离子源,正离子模式,多反应监测模式检测,基质匹配工作曲线外标法定量.灭螨醌和羟基灭螨醌在0.200~20.0 ng/mL范围内线性良好,相关系数均大于0.999.灭螨醌检出限为1.25 μg/kg,羟基灭螨醌检出限为0.5 μg/kg;灭螨醌定量限为4 μg/kg,羟基灭螨醌定量限为2 μg/kg.灭螨醌和羟基灭螨醌三水平的加标回收率为77.0%~100.2%,相对标准偏差1.7%~7.8%.该方法操作简便、快速准确,适用于茶叶中灭螨醌及其代谢物的批量测定.
Determination of Acaroquinone and Its Metabolites in Tea by Modified SinChERS Combined with Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry
A detection method based on SinChERS purification technology combined with ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was established to determine the residual levels of acaricide quinone and its metabolite hydroxy acaricide quinone in tea.The sample was extracted by 1%formic acid acetonitrile,purified by SinChERS-TPR,separated by Agilent C18 chromatographic column,gradient eluted with 0.1%formic acid water and methanol as mobile phase,detected by electrospray ion(ESI)source,positive ion mode,multiple reaction monitoring(MRM)mode,and quantified by matrix matching working curve external standard method.The linear relationship between acaroquinone and hydroxy acaroquinone exhibited good linearity in the range of 0.200 ng/mL to 20.0 ng/mL,with correlation coefficients greater than 0.999.The limit of detection for acariquinone was 1.25μg/kg,and for hydroxy acaroquinone was limited to 0.50 μg/kg;the limit of quantitation for acaroquinone was 4 μg/kg,and for the hydroxy acaroquinone was 2 pg/kg.The recovery rates of the three levels of acaroquinone and hydroxy acaroquinone were 77.0%to 100.2%,with a relative standard deviation of 1.7%to 7.8%.This method was easy to operate,fast and accurate,and was suitable for batch determination of acaroquinone and its metabolites in tea.

acaroquinonehydroxy acaroquinoneteaSinChERS

苏敏、钟世欢、王静、叶佳明、黄南、杨天明、陆梅阳

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浙江公正检验中心有限公司,浙江杭州 310000

浙江省食品安全重点实验室,浙江杭州 310000

灭螨醌 羟基灭螨醌 茶叶 SinChERS

浙江省自然科学基金项目赞宇科研基金项目

LTGC24B0500112024005

2024

食品科技
北京市粮食科学研究所

食品科技

CSTPCD北大核心
影响因子:0.622
ISSN:1005-9989
年,卷(期):2024.49(7)