固相萃取-液相色谱-串联质谱法检测小鼠肌肉组织中矮壮素  

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

作　　者：李春梅[1,2] 金芬[1] 徐思远[1] 刘佳佳[1,3] 金茂俊[1] 邵华[1] 王静[1] 杨鸣琦[2] 

机构地区：[1]中国农业科学院农产品质量与食物安全重点实验室 农业质量标准与检测技术研究所,北京100081 [2]西北农林科技大学动物医学院,杨凌712100 [3]中粮营养健康研究院,北京100083

出　　处：《分析化学》2012年第12期1924-1928,共5页Chinese Journal of Analytical Chemistry

基　　金：国家自然基金资助项目(No.21107138)

摘　　要：建立了快速检测小鼠肌肉组织中矮壮素的固相萃取-液相色谱-串联质谱(SPE-LC-MS/MS)方法。小鼠肌肉样品经乙腈提取,弱阳离子交换(WCX)固相萃取柱净化,3 mL甲酸-甲醇(1∶99,V/V)重力洗脱。采用亲水作用色谱柱(HILIC),含10 mmol/L乙酸铵、0.1%甲酸水溶液-乙腈(40∶60,V/V)为流动相,以电喷雾正离子(ESI+)、多反应监测模式(MRM)进行矮壮素的定性分析,采用基质标准曲线外标法进行定量分析。结果表明:矮壮素的线性范围为5.0～500.0μg/L,线性相关系数为0.9991。在10.0,100.0和200.0μg/kg添加浓度下的回收率为73.2%～82.3%;相对标准偏差小于9.3%;方法定量限为10.0μg/kg,能够满足小鼠肌肉组织中痕量矮壮素检测的要求。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.

关 键 词：液相色谱-串联质谱 矮壮素 肌肉 弱阳离子交换固相萃取 

分 类 号：Q593.3[生物学—生物化学] O657.63[理学—分析化学]