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一种通用、快速测定茶叶中农药和真菌毒素的新型样品前处理方法,采用超高效液相色谱-串联质谱法。

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.

机构信息

Ningbo Academy of Inspection and Quarantine, Ningbo 315012, China.

Laboratory for Managing Biotic and Chemical Threats to the Quality and Safety of Agro-products, School of Marine Sciences, Ningbo University, Ningbo 315211, China.

出版信息

J Chromatogr A. 2021 Jan 11;1636:461794. doi: 10.1016/j.chroma.2020.461794. Epub 2020 Dec 11.

Abstract

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 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 μg/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 ta 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.

摘要

建立了一种快速、简单、通用的分析方法,用于同时测定红茶中 140 种不同化学类别的不良低分子量农药和真菌毒素。该方法涉及在乙酸铵缓冲液中使样品溶胀,用乙腈-二甲基亚砜提取,在低温离心的辅助下用双分散固相萃取(D-SPE)进行净化,并用超高效液相色谱-电喷雾串联质谱法(MS/MS)在多反应监测模式下进行分析。通过仅使用 C 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,从而长时间保持色谱柱处于理想状态,同时实现了亲水性和疏水性分析物的满意回收。大多数目标化合物的基质匹配校准曲线的线性回归系数均大于 0.9900。定量限(LOQ)的范围在 0.5-10.0μg/kg 内,通常足以验证产品是否符合法定公差。在红茶样品中的回收率为 64.5%-138.1%,相对标准偏差(RSD)值在 1.8%-25.9%之间。日间精密度的范围在 2.2%-24.9%之间。对于超过 90%的分析物,回收率在 70%-120%之间,RSD 值低于 15.0%。该方法在常规监测计划中的应用可以大大减少工作量和时间。

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