Rapid determination of chlormequat in meat by dispersive solid-phase extraction and hydrophilic interaction liquid chromatography (HILIC)-electrospray tandem mass spectrometry.
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.
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.
Chunmei
C
Li
Fen
F
Jin
Zhiyong
Z
Yu
Yamei
Y
Qi
Xiaomei
X
Shi
Miao
M
Wang
Hua
H
Shao
Maojun
M
Jin
Jing
J
Wang
Mingqi
M
Yang
D000818:Animals; D002417:Cattle; D002645:Chickens; D002681:China; D002716:Chlormequat / Q000032:analysis* / Q000302:isolation & purification*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D005506:Food Contamination / Q000032:analysis; D006041:Goats; D008460:Meat / Q000032:analysis*; D010937:Plant Growth Regulators / Q000032:analysis* / Q000302:isolation & purification*; D052616:Solid Phase Extraction / Q000379:methods*; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods; D013552:Swine; D053719:Tandem Mass Spectrometry / Q000379:methods*
D010937:Plant Growth Regulators; D002716:Chlormequat