Simultaneous quantification of mycotoxins and pesticide residues in ginseng with one-step extraction using ultra-high performance liquid chromatography-electrospray ionization tandem mass spectrometry
Simultaneous quantification of mycotoxins and pesticide residues in ginseng with one-step extraction using ultra-high performance liquid chromatography-electrospray ionization tandem mass spectrometry
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DOI：
10.1016/j.jchromb.2013.09.013
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发表时间：
2013-11-15
影响因子：
3
通讯作者：
Yang, Meihua
中科院分区：
文献类型：
--
作者：
Kuang, Ying;Qiu, Feng;Yang, Meihua
建立了一种简便、准确、灵敏的超高效液相色谱-电喷雾串联质谱（UHPLC-ESI-MS/MS）同时测定人参中10种真菌毒素和29种农药残留的方法。该方法采用乙腈/水/甲酸（99：33：1，v/v/v）快速简单的一步萃取程序，无需进一步净化。在Phenomenex Kinetex C-18柱（2.1 mm × 100 mm，2.6 μ m）上，以0.30 mL/min的流速，使用含有0.1%甲酸和甲醇的水的移动的流动相，成功地在8 min内实现快速LC分离。在正离子和负离子模式下进行同时采集。对于一些分析物，在负离子模式下获得增强的响应（例如，玉米赤霉烯酮、α-玉米赤霉烯醇和β-玉米赤霉烯醇）;然而，大多数分析物在正离子模式下通过多反应监测（MRM）进行监测。采集每种分析物的两次MS/MS跃迁，以确保可靠的鉴别和准确的定量。通过线性、选择性、精密度和回收率研究，在内部对该方法进行了验证。分析数据令人满意，典型回收率为70-120%，相对标准偏差（RSD）低于20%。检测限（LOD）范围为0.01至0.25 ng/mL，低于欧洲食品和食品中真菌毒素或农药法规规定的最大残留水平（MRL）。从中国市场采集的43个人参样品（人参30个、西洋参6个、红参7个）中，检出率最高的农药是毒死蜱，检出率为97%，含量范围为37.63 ~ 158.60 μ g/kg。还将离子比、保留时间和实验Q/q比与相应参比标准品进行了比较，以避免假阳性结果。(C)2013 Elsevier B. V.保留所有权利。
This study describes the development and validation of a simple, accurate and sensitive ultra high-performance liquid chromatography-electrospray ionization tandem mass spectrometry (UHPLC-ESI-MS/MS) method for the simultaneous quantification of 10 mycotoxins and 29 pesticides in ginseng. The method featured a fast and straightforward one-step extraction procedure using acetonitrile/water/formic acid (99:33:1, v/v/v) without further cleanup. Rapid LC separation in 8 min was successfully achieved on a Phenomenex Kinetex C-18 column (2.1 mm x 100 mm, 2.6 mu m) with a flow rate of 0.30 mL/min using a mobile phase of water containing 0.1% formic acid and methanol. Simultaneous acquisition was performed in the positive and negative ion modes. For some analytes, enhanced responses were acquired in negative ion mode (e.g., Zearalenone, alpha-Zearalenol and beta-Zearalenol); however, the majority of analytes were monitored in positive ion mode with multiple reaction monitoring (MRM). Two MS/MS transitions for each analyte were acquired to ensure reliable identification and accurate quantification. The method was validated in house through linearity, selectivity, precision, and recovery studies. Analytical data were satisfactory with typical recoveries of 70-120% and relative standard deviations (RSDs) below 20%. The limits of detection (LODs) ranged from 0.01 to 0.25 ng/mL, which are below the maximum residue levels (MRLs) established by European legislation for mycotoxins or pesticides in foods and foodstuffs. Forty-three ginseng samples (ginseng (n = 30), American ginseng (n = 6), red ginseng (n = 7)) collected from Chinese markets were analyzed and the most frequently detected pesticide was chlorpyrifos with an incidence of 97% and ranged from 37.63 to 158.60 mu g/kg. Ion ratios, retention times and experimental Q/q ratios were also compared with those of the corresponding reference standard in order to avoid false-positive results. (C) 2013 Elsevier B.V. All rights reserved.