On-line liquid chromatography-mass spectrometry with dilution line to achieve large volume urine injection for the improvement of sensitivity

CORC > 生态环境研究中心 > 中国科学院生态环境研究中心 > 环境化学与生态毒理学国家重点实验室

	On-line liquid chromatography-mass spectrometry with dilution line to achieve large volume urine injection for the improvement of sensitivity
	Liu, Min; Yan, Wei; Lin, Jin-Ming; Hashi, Yuki; Liu, Li-bin; Wei, Yanlin
刊名	JOURNAL OF CHROMATOGRAPHY A
	2008-07-11
卷号	1198 期号:1 页码:87-94
关键词	large volume injection dilution line on-line liquid chromatography-mass spectrometry estrogens spiked urine samples
英文摘要	A unique automated on-line high-performance liquid chromatography-mass spectrometry (LC-MS) method was developed allowing injection of a large volume of urine for the improvement of sensitivity using estrogens as analytes. The urine sample was precipitated by acetonitrile (sample: acetonitrile, 1 :2, v/v) to remove most proteins. Then the supernatant was directly delivered at 0.3 mL/min by a pump, which broke through the limit of autosampler with fixed loop. Then the sample was loaded onto a restricted access media (RAM) pre-column after on-line dilution with NH4Ac solution which was delivered by another pump under high flow-rate. After the addition of on-line dilution line, the content of organic solvent in the sample aliquot was sharply decreased so that the analytes were effectively trapped by pre-column. In addition, another 6-port valve was added to selectively deliver the effluent containing analytes into MS, which minimized the pollution of the MS and matrix effect. After optimization of the condition of extraction method, 3 mL sample (containing I mL urine) could be successfully enriched. The injection volume increased 10 times compared with conventional on-line LC-MS methods for biofluid analysis, significantly improving sensitivity. Moreover, no obvious increase of column pressure was observed after 300 injections. The method was validated by spiking urine. Linearity was determined by sample which was in the range of 1-500 ng/mL. The process efficiency ranged from 70.2 to 106% with RSDs less than 15% with the exception of a few analytes. The limit of detection (LOD) and quantification (LOQ) ranged from 0.3 to 2 ng/mL and 1 to 8 ng/mL, respectively, corresponding a decrease of 1-2 orders of magnitude compared with those of off-line and on-line methods. (c) 2008 Elsevier B.V. All rights reserved.
WOS记录号	WOS:000257545600014
内容类型	期刊论文
源URL	[http://ir.rcees.ac.cn/handle/311016/21966]
专题	生态环境研究中心_环境化学与生态毒理学国家重点实验室
推荐引用方式 GB/T 7714	Liu, Min,Yan, Wei,Lin, Jin-Ming,et al. On-line liquid chromatography-mass spectrometry with dilution line to achieve large volume urine injection for the improvement of sensitivity[J]. JOURNAL OF CHROMATOGRAPHY A,2008,1198(1):87-94.
APA	Liu, Min,Yan, Wei,Lin, Jin-Ming,Hashi, Yuki,Liu, Li-bin,&Wei, Yanlin.(2008).On-line liquid chromatography-mass spectrometry with dilution line to achieve large volume urine injection for the improvement of sensitivity.JOURNAL OF CHROMATOGRAPHY A,1198(1),87-94.
MLA	Liu, Min,et al."On-line liquid chromatography-mass spectrometry with dilution line to achieve large volume urine injection for the improvement of sensitivity".JOURNAL OF CHROMATOGRAPHY A 1198.1(2008):87-94.