Rapid Determination of Chlormequat in Meat by Dispersive Solid-Phase Extraction and Hydrophilic Interaction Liquid Chromatography (HILIC)鈥揈lectrospray Tandem Mass Spectrometry
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- 作者：Chunmei Li ; Fen Jin ; Zhiyong Yu ; Yamei Qi ; Xiaomei Shi ; Miao Wang ; Hua Shao ; Maojun Jin ; Jing Wang ; Mingqi Yang
- 刊名：Journal of Agricultural and Food Chemistry
- 出版年：2012
- 出版时间：July 11, 2012
- 年：2012
- 卷：60
- 期：27
- 页码：6816-6822
- 全文大小：345K
- 年卷期：v.60,no.27(July 11, 2012)
- ISSN：1520-5118
文摘
A rapid method for analyzing trace levels of chlormequat (CQ) in meat samples by hydrophilic interaction liquid chromatography (HILIC)鈥揺lectrospray 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鈥?00 渭g/L. The limit of detection (LOD) was estimated at 0.03 渭g/kg for CQ on the basis of a peak to peak signal noise (S/N = 3). The limit of quantification (LOQ) was 0.1 渭g/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鈥?4.7% at 2, 20, and 200 渭g/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鈥?36.0 渭g/kg. Concentrations in a chicken sample (636.0 渭g/kg) and a goat meat sample (486.0 渭g/kg) were found to be 15.9 and 2.43 times the corresponding Codex maximum residue limits, respectively.