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A novel sample-preparation method for the generic and rapid determination of pesticides and mycotoxins in tea by ultra-performance liquid chromatography-tandem mass spectrometry

机译:一种新的样品制备方法,用于通过超高效液相色谱 - 串联质谱法进行粉体粉药和霉菌毒素的通用和快速测定方法

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摘要

A rapid, simple, and generic analytical method for the simultaneous determination of 140 undesirable low-weight pesticides and mycotoxins from different chemical classes in black tea was developed. The method involved swelling the sample in ammonium acetate buffer, extraction with acetonitrile-dimethyl sulfoxide, cleanup by dual dispersive solid-phase extraction (D-SPE) with the assistance of low-temperature centrifugation, and analysis by ultraperformance liquid chromatography coupled with electrospray ionization tandem mass spectrometry using multiple reaction monitoring mode. The interferences in the extract were eliminated by the combination of dual D-SPE using only C-18 sorbent and anhydrous magnesium sulfate, which maintained the chromatographic column under the ideal condition for a long time and enabled satisfactory recoveries of hydrophobic and hydrophilic analytes simultaneously. Matrix-matched calibration curves were obtained for most target compounds with linear regression coefficients above 0.9900. The limits of quantification (LOQs) ranged within 0.5-10.0 Ag/kg, which were usually sufficient to verify the compliance of products with legal tolerances. Satisfactory recoveries of 64.5%-138.1% were obtained in black to samples with the relative standard deviation (RSD) values between 1.8 and 25.9%. The inter-day precision ranged within 2.2%-24.9%. For over 90% of the analytes, the recoveries were between 70% and 120%, with RSD values below 15.0%. The application of this method in routine monitoring programs can drastically reduce effort and time. (C) 2020 Elsevier B.V. All rights reserved.
机译:建立了一种快速、简便、通用的分析方法,可同时测定红茶中不同化学类别的140种不良低量农药和真菌毒素。该方法包括在醋酸铵缓冲液中溶胀样品,用乙腈-二甲基亚砜萃取,在低温离心的帮助下通过双分散固相萃取(D-SPE)进行净化,以及使用多反应监测模式通过超高效液相色谱与电喷雾电离串联质谱联用进行分析。通过仅使用C-18吸附剂和无水硫酸镁的双D-SPE组合,消除了提取物中的干扰,从而使色谱柱长时间保持在理想条件下,同时实现了疏水性和亲水性分析物的满意回收。对于大多数线性回归系数大于0.9900的目标化合物,获得了基质匹配校准曲线。定量限(LOQ)在0.5-10.0 Ag/kg范围内,通常足以验证产品是否符合法定公差。样品的相对标准偏差(RSD)在1.8%到25.9%之间,黑色样品的回收率为64.5%-138.1%。日间精密度在2.2%-24.9%之间。对于超过90%的分析物,回收率在70%到120%之间,RSD值低于15.0%。在常规监测项目中应用这种方法可以大大减少工作量和时间。(C) 2020爱思唯尔B.V.版权所有。

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