Citation: LI Chun-Mei, JIN Fen, XU Si-Yuan, LIU Jia-Jia, JIN Mao-Jun, SHAO Hua, WANG Jing, YANG Ming-Qi. Determination of Chlormequat in Muscles of Mice by Solid Phase Extraction-Liquid Chromatography-Tandem Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, ;2012, 40(12): 1924-1928. doi: 10.3724/SP.J.1096.2012.20371 shu

Determination of Chlormequat in Muscles of Mice by Solid Phase Extraction-Liquid Chromatography-Tandem Mass Spectrometry

LI Chun-Mei ^1,2 ,
JIN Fen ^1,, ,
XU Si-Yuan ¹ ,
LIU Jia-Jia ^1,3 ,
JIN Mao-Jun ¹ ,
SHAO Hua ¹ ,
WANG Jing ¹ ,
YANG Ming-Qi ^2,,

1.
¹ Key Lab of Agro-product Quality and Safety, Institute of Quality Standards & Testing Technology for Agro-products, Chinese Academy of Agricultural Sciences, Beijing 100081, China;

Corresponding author: JIN Fen, YANG Ming-Qi,
Received Date: 9 April 2012
Available Online: 17 July 2012
Fund Project: 本文系国家自然基金资助项目(No.21107138) (No.21107138)

A method for the determination of chlormequat (CQ) in muscles of mice using solid phase extraction with liquid chromatography tandem mass spectrometry was developed. CQ was extracted using acetonitrile, cleaned-up by Weak Cation-exchange (WCX) solid phase extraction (SPE) cartridges and then eluted by 3 mL of formic acid-methanol (1:99, V/V) by gravity. The separation was performed on a hydrophilic interaction liquid chromatography (HILIC) column with aqueous solution containing 10 mmol/L ammonium acetate and 0.1% formic acid-acetonitrile (40:60, V/V) as the mobile phase. CQ was determined in the mode of electrospray ionization source (ESI⁺) and multiple-reaction monitoring (MRM). The quantification was carried out by matrix-matched external standard curve. The results showed that the calibration curve was linear in the range of 5.0-500.0 μg/L with the correlation coefficient of 0.9991. The mean recovery of CQ in spiked muscle samples was 73.2%-82.3% and the relative standard deviation (RSD) was less than 9.3% at 10.0, 100.0 and 200.0 μg/kg with three spiked levels (n=7). The limit of quantification (LOQ) for CQ was 10.0 μg/kg. The method was successfully applied to the analysis of trace level of CQ in muscles of mice.
- Liquid chromatography-mass spectrometry,
- Chlormequat,
- Muscles,
- Weak cation exchange solid phase extraction
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