分析测试学报2011，Vol.30Issue(3)：321-325,5.DOI:10.3969/j.issn.1004-4957.2011.03.018
高效液相色谱-串联质谱法测定食品中的矮壮素与缩节胺残留
Determination of Chlormequat and Mepiquat Residues in Food by High Performance Liquid Chromatography- Tandem Mass Spectrometry
摘要
Abstract
A high performance liquid chromatography -electrospray ionization tandem mass spectrometric( HPLC -ESI MS/MS) method was developed for the determination of two plant growth regulators, e.g. chlormequat and mepiquat, in rice, wheat flour, pear, tomato and ketchup samples. The samples were extracted with methanol- water( 1 : 1, by volume) and cleaned up on a Strata-X-C solid-phase extraction column. The target compounds were separated on an Agilent ZORBAX RXSIL( 1.8 μm, 3.0 mm × 100 mm) chromatographic column by equivalently elution using acetronitrilie - 10 mmoL/L ammonium acetate( containing O. 1％ formic acid ) as mobile phase. The residues of chlormequat and mepiquat were determined under the electrospray positive ionization( ESI + ) and multiple reaction monitoring (MRM) mode, and quantified by the matrix-matched external standard method. The calibration curves for chlormequat and mepiquat showed good linearities in the range of O. 20 - 10 μg/L with correlation coefficients ( r2 ) no less than 0. 999 0. The limits of quantitation ( S/N≥ 10) and limits of detection( S/N≥3 ) were in the range of 0. 05 - O. 15 μg/kg and 0. 02 - 0. 05 μg/kg, respectively. The average recoveries of chlormequat and mepiquat from rice, wheat flour, pears, tomato and ketchup matries at three spiked levels of O. 20, 5. O, 10 μg/kg were in the range of 82％ - 102％ and 80％ - 103％ , respectively, with relative standard deviations of 3.8％ - 9. 6％ and 1.9％ -10.0％ , respectively. The method was sensitive and accurate, and could meet the requirements for the determination of chlormequat and mepiquat in foods.关键词
矮壮素/缩节胺/高效液相色谱/串联质谱/食品Key words
chlormequat/ mepiquat/ HPLC/ tandem mass spectrometry/ food分类
化学化工引用本文复制引用
鲁立良,罗小玲,王远,郝家勇..高效液相色谱-串联质谱法测定食品中的矮壮素与缩节胺残留[J].分析测试学报,2011,30(3):321-325,5.基金项目
新疆农垦科学院青年基金资助项目(YQJ2009-11) （YQJ2009-11）
