[1]谢巧珍,皋伟,李季峰,等.头发中内源性氢化可的松的高效液相色谱／串联质谱检测[J].东南大学学报(自然科学版),2011,41(3):579-583.[doi:10.3969/j.issn.1001-0505.2011.03.029]
　Xie Qiaozhen,Gao Wei,Li Jifeng,et al.Detection of endogenous cortisol in human hair by high performance liquid chromatography tandem mass spectrometry[J].Journal of Southeast University (Natural Science Edition),2011,41(3):579-583.[doi:10.3969/j.issn.1001-0505.2011.03.029]
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头发中内源性氢化可的松的高效液相色谱／串联质谱检测()
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《东南大学学报(自然科学版)》[ISSN:1001-0505/CN:32-1178/N]

卷:
41
期数:
2011年第3期
页码:
579-583
栏目:
环境科学与工程
出版日期:
2011-05-20

文章信息/Info

Title:
Detection of endogenous cortisol in human hair by high performance liquid chromatography tandem mass spectrometry
作者:
谢巧珍; 皋伟; 李季峰; 乔婷; 邓慧华; 陆祖宏
(东南大学学习科学研究中心儿童发展与学习科学教育部重点实验室, 南京 210096)
(东南大学学习科学研究中心, 南京 210096)
Author(s):
Xie Qiaozhen; Gao Wei; Li Jifeng; Qiao Ting; Deng Huihua; Lu Zuhong
(Key Laboratory of Child Development and Learning Science of Ministry of Education, Southeast University, Nanjing 210096, China)
(Research Center of Learning Science, Southeast University, Nanjing 210096, China)
关键词:
高效液相色谱/串联质谱; 氢化可的松; 头发; 高效液相色谱/荧光法
Keywords:
high performance liquid chromatography tandem mass spectrometry;  cortisol;  hair;  high performance liquid chromatography with fluorescence detector
分类号:
X703
DOI:
10.3969/j.issn.1001-0505.2011.03.029
摘要:
基于高效液相色谱/串联质谱(HPLC/MS/MS)建立了一种检测头发中内源性氢化可的松含量的方法,并与高效液相色谱/荧光法(HPLC/FLU)的测定结果进行比较.头发样品(50 mg)经过清洗与研磨、甲醇提取和 C18 固相萃取后,在电喷雾(ESI)负离子模式和多反应监测(MRM)方式下进行定性,以外标法进行定量.方法的定量限为2 pg/mg,工作曲线的线性范围为2~100 pg/mg; 在空白头发添加50 pg/mg外标时,方法的回收率为(99.4±9.1)%,日内精密度为7.6%,日间精密度为8.3%.由于前处理提取方法、基质效应和定量方法不同,所以HPLC/MS/MS法的测定结果明显低于HPLC/FLU法的测定结果.尽管如此,皮尔逊相关性分析发现2种方法测定的结果具有显著相关性(r=0.749,p<0.01).
Abstract:
A new method for detection of endogenous cortisol in human hair was developed based on high performance liquid chromatography tandem mass spectrometry (HPLC/MS/MS), and the results detected was compared with that determined by high performance liquid chromatography with fluorescence detector (HPLC/FLU). Hair sample (50 mg) was incubated in methanol after being washed and pulverized, and then the extraction was purified by C18 solid phase extraction column. Cortisol identification was performed by electro-spray ionization (ESI) in negative mode using multiple reaction monitoring (MRM) and the quantification was performed using external standard method. The limit of quantification is 2 pg/mg, and the linear range is 2 to 100 pg/mg. The recovery of cortisol spiked at 50 pg/mg is (99. 4±9. 1)%, intra-day precision is 7. 6%, inter-day precision is 8. 3%. Because of the differences in hair pretreatment method, cortisol extraction method, matrix effect and quantitative method, cortisol concentration detected by HPLC/MS/MS is significantly lower than that determined by HPLC/FLU. However, Pearson correlation analysis showed that there is a significant linear correlation (r=0. 749, p<0. 01) between hair cortisol contents analyzed by these two methods.

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备注/Memo

备注/Memo:
作者简介:谢巧珍(1986—),女,硕士生;邓慧华(联系人),男,博士,教授,博士生导师,dengrcls@seu.edu.cn.
基金项目:国家自然科学基金资助项目(60771023)、教育部新世纪人才计划资助项目(NCET-08-0122)、江苏省社会科学基金重点资助项目(09IYA002)、东南大学博士生创新基金资助项目(BC0905).
引文格式: 谢巧珍,皋伟,李季峰,等.头发中内源性氢化可的松的高效液相色谱/串联质谱检测[J].东南大学学报:自然科学版,2011,41(3):579-583.[doi:10.3969/j.issn.1001-0505.2011.03.029]
更新日期/Last Update: 2011-05-20