Changchun Centre of Mass Spectrometry, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Changchun 130022, China.
J Chromatogr A. 2012 Feb 17;1225:132-40. doi: 10.1016/j.chroma.2011.12.071. Epub 2011 Dec 30.
An ultra-high-performance liquid chromatographic-tandem mass spectrometry (UHPLC-MS/MS) method for the simultaneous quantification and identification of 116 pesticide residues which were most widely used in plants used in Traditional Chinese Medicine (TCM) in 15 min has been developed and validated. Samples were extracted and cleaned up with modified QuEChERS method and detected by UHPLC-MS/MS under multiple reactions monitoring mode, and quantified by matrix-match calibration. The validation study was carried out on five different matrixes following DG SANCO/2007/3131 of the European Quality Control Guidelines. The linearity of the calibration was good between 5 and 100 ng ml⁻¹ concentration ranges, and the limits of quantification (LOQs) less than 0.01 mg/kg for most pesticides. The mean recoveries of almost all pesticides were in the range from 70% to 120% at three concentration levels ranging from 0.01 mg/kg to 0.1mg/kg with relative standard deviations (RSD) better than 15%. The method was applied on 138 real samples from 102 different kinds of Chinese herbal medicine. 95 positive samples were detected. This method is fast, robust, accurate, selective, sensitive and easy to operate.
建立并验证了一种超高效液相色谱-串联质谱（UHPLC-MS/MS）方法，用于在 15 分钟内同时定量和鉴定 116 种农药残留，这些农药残留是在中药材中最广泛使用的。样品采用改良的 QuEChERS 方法提取和净化，在多反应监测模式下通过 UHPLC-MS/MS 检测，并通过基质匹配校准定量。验证研究遵循欧洲质量控制指南 DG SANCO/2007/3131 ，在五种不同基质上进行。校准的线性在 5 至 100ng/ml 浓度范围内良好，大多数农药的定量限（LOQ）小于 0.01mg/kg。在 0.01mg/kg 至 0.1mg/kg 的三个浓度水平范围内，几乎所有农药的平均回收率均在 70%至 120%范围内，相对标准偏差（RSD）优于 15%。该方法应用于来自 102 种不同中药材的 138 个实际样品，检测到 95 个阳性样品。该方法快速、稳健、准确、选择性好、灵敏度高且易于操作。
