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首页> 美国卫生研究院文献>Journal of Advanced Research >A modified QuEChERS method coupled with liquid chromatography-tandem mass spectrometry for the simultaneous detection and quantification of scopolamine L-hyoscyamine and sparteine residues in animal-derived food products
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A modified QuEChERS method coupled with liquid chromatography-tandem mass spectrometry for the simultaneous detection and quantification of scopolamine L-hyoscyamine and sparteine residues in animal-derived food products

机译：改进的QuEChERS方法与液相色谱-串联质谱联用可同时检测和定量动物源食品中东pol碱L-hycycyamine和sparteine残留

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class="kwd-title">Keywords: Scopolamine, L-hyoscyamine, Sparteine, Porcine muscle, Egg, Milk, QuEChERS, Residues, LC-MS/MS class="head no_bottom_margin" id="ab015title">AbstractWe developed a modified Quick, Easy, Cheap, Effective, Rugged, and Safe (CEN QuEChERS) extraction method coupled with liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI+/MS-MS) to identify and quantify residues of three botanical alkaloids, namely, scopolamine, L-hyoscyamine, and sparteine, in animal-derived foods, including porcine muscle, egg, and milk. A combination of ethylenediaminetetraacetic acid disodium buffer and acetonitrile acidified with 0.5% trifluoroacetic acid was used as an extraction solvent, whereas QuEChERS (CEN, 15662) kits and sorbents were applied for cleanup procedures. The proposed method was validated by determining the limits of quantification (LOQs), with values of 1–5 µg/kg achieved for the target analytes in various matrices. Linearity was estimated from matrix-matched calibration curves constructed using six concentration levels ranging from 1- to 6-fold increases in the LOQs of each analyte, and the correlation coefficients (R2) were ≥0.9869. Recoveries (at three concentration levels of 1-, 2-, and 3-fold increases in the LOQ) of 73–104% were achieved with relative standard deviations (RSDs) ≤7.7% (intra-day and inter-day precision). Ten types of each matrix procured from large markets were evaluated, and all tested samples showed negative results. The current protocol is simple and versatile and can be used for routine detection of plant alkaloids in animal food products.
机译：<！-fig ft0-> <！-fig @ position =“ anchor” mode =文章f4-> <！-fig mode =“ anchred” f5-> <！-fig / graphic | fig / alternatives / graphic mode =“ anchored” m1-> class =“ kwd-title”>关键字： Scopolamine，L-hycycyamine，Sparteine，猪肌肉，鸡蛋，牛奶，QuEChERS，残留物，LC- MS / MS class =“ head no_bottom_margin” id =“ ab015title”>摘要我们开发了一种改进的快速，简便，廉价，有效，坚固而安全的提取方法（CEN QuEChERS），并结合了液相色谱-电喷雾电离串联质谱（LC-ESI + / MS-MS）来鉴定和定量动物源性食品（包括猪）中三种植物生物碱（东碱，L-hycycyamine和sparteine）的残留量肌肉，鸡蛋和牛奶。乙二胺四乙酸二钠缓冲液和用0.5％三氟乙酸酸化的乙腈的组合用作萃取溶剂，而QuEChERS（CEN，15662）试剂盒和吸附剂用于清洁程序。通过确定定量限（LOQs）验证了所提出的方法，在各种基质中目标分析物的定量限值为1-5 µg / kg。线性是根据基质匹配的校准曲线估算的，该校准曲线使用六个浓度水平（每种分析物的LOQ增加1至6倍）构建，相关系数（R 2 ）≥0.9869。相对标准偏差（RSD）≤7.7％（日内和日间精度），回收率（LOQ浓度分别增加1、2和3倍的三个浓度水平）达到73-104％。对从大型市场采购的每种基质的十种类型进行了评估，所有测试样品均显示阴性结果。当前的协议既简单又通用，可用于动物食品中植物生物碱的常规检测。

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