Key Laboratory of Agro-product Quality and Safety, Institute of Quality Standards and Testing Technology for Agro-products, Chinese Academy of Agricultural Sciences , Beijing 100081, China.
J Agric Food Chem. 2012 Jul 11;60(27):6816-22. doi: 10.1021/jf3010756. Epub 2012 Jun 25.
A rapid method for analyzing trace levels of chlormequat (CQ) in meat samples by hydrophilic interaction liquid chromatography (HILIC)-electrospray tandem mass spectrometry was developed. The samples were extracted with acetonitrile, followed by a rapid cleanup through a dispersive solid-phase extraction (DSPE) technique with octadecyl (C18) DSPE sorbents. The chromatographic separation was achieved within 6 min using a HILIC column with 10 mM ammonium acetate and 0.1% (v/v) formic acid in water/acetonitrile (v/v, 40:60) as the mobile phase. Quantification was performed using a matrix-matched calibration curve, which was linear in the range of the 0.05-100 μg/L. The limit of detection (LOD) was estimated at 0.03 μg/kg for CQ on the basis of a peak to peak signal noise (S/N = 3). The limit of quantification (LOQ) was 0.1 μg/kg on the basis of the lowest spiked concentration with suitable precision and accuracy. The average recovery of CQ in spiked meat samples was 86.4-94.7% at 2, 20, and 200 μg/kg. Finally, this method was applied to determine CQ in the livestock and poultry meats purchased from markets in Beijing in 2011. CQ was detected in all 12 samples, and the concentration was 0.4-636.0 μg/kg. Concentrations in a chicken sample (636.0 μg/kg) and a goat meat sample (486.0 μg/kg) were found to be 15.9 and 2.43 times the corresponding Codex maximum residue limits, respectively.
建立了一种通过亲水作用色谱-电喷雾串联质谱法（HILIC-ESI-MS/MS）快速分析肉样中痕量氯喹（CQ）的方法。样品用乙腈提取，然后通过十八烷基（C18）DSPE 吸附剂的分散固相萃取（DSPE）技术进行快速净化。使用 HILIC 柱，以 10 mM 乙酸铵和 0.1%（v/v）甲酸的水/乙腈（v/v，40:60）为流动相，在 6 min 内实现色谱分离。采用基质匹配校准曲线进行定量，CQ 在 0.05-100 μg/L 范围内呈线性。以峰峰信号噪声（S/N = 3）为基础，CQ 的检测限（LOD）估计为 0.03 μg/kg。基于合适的精密度和准确度，以最低加标浓度为基础，定量限（LOQ）为 0.1 μg/kg。在 2、20 和 200 μg/kg 的加标浓度下，CQ 在加标肉样中的平均回收率为 86.4-94.7%。最后，该方法应用于 2011 年在北京市场购买的畜禽肉中 CQ 的测定。在所有 12 个样品中均检测到 CQ，浓度为 0.4-636.0 μg/kg。在一个鸡肉样品（636.0 μg/kg）和一个山羊肉样品（486.0 μg/kg）中的浓度分别是相应的食品法典最大残留限量的 15.9 和 2.43 倍。
