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

引用本文: 李春梅, 金芬, 徐思远, 刘佳佳, 金茂俊, 邵华, 王静, 杨鸣琦. 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[J]. 分析化学, 2012, 40(12): 1924-1928. doi: 10.3724/SP.J.1096.2012.20371 shu

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

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

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,
,}

通讯作者: 金芬,杨鸣琦; 金芬,杨鸣琦

基金项目:
本文系国家自然基金资助项目(No.21107138) (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5.0-500.0 μg/L,线性相关系数为0.9991。在10.0,100.0和200.0 μg/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10.0 μg/kg,能够满足小鼠肌肉组织中痕量矮壮素检测的要求。

关键词:

English

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

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: 金芬,杨鸣琦; 金芬,杨鸣琦

Received Date: 09 April 2012
Fund Project:
本文系国家自然基金资助项目(No.21107138)

Abstract: 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.

Key words:

Liquid chromatography-mass spectrometry
/ Chlormequat
/ Muscles
/ Weak cation exchange solid phase extraction

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1.
沈阳化工大学材料科学与工程学院沈阳 110142

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

通讯作者: 金芬,杨鸣琦; 金芬,杨鸣琦

English

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

Corresponding author: 金芬,杨鸣琦; 金芬,杨鸣琦

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

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

通讯作者: 金芬,杨鸣琦; 金芬,杨鸣琦

English

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

Corresponding author: 金芬,杨鸣琦; 金芬,杨鸣琦

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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通讯作者: 陈斌, bchen63@163.com

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