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DOI10.3724/SP.J.1123.2010.00197
Simultaneous determination of trace diphacinone and chlorophacinone in biological samples by high performance liquid chromatography coupled with ion trap mass spectrometry
Jin Micong; Chen Xiaohong
通讯作者Jin, MC
来源期刊CHINESE JOURNAL OF CHROMATOGRAPHY
ISSN1000-8713
出版年2010
卷号28期号:2页码:197-203
英文摘要A rapid qualitative and quantitative method for the simultaneous determination of trace diphacinone and chlorophacinone in biological samples has been established. The method mainly serves for the emergent poisoning detection. The whole blood was treated with methanol-acetonitrile (50/50, v/v) and the urine was cleaned-up by Waters Oasis HLB SPE cartridges. The samples were separated on an Extend C18 column (150 mm x 4.6 mm, 5 mu m) by using the mobile phase consisted of ammonium acetate-acetic acid (0.02 mol/L, pH 5.5)-methanol (15/85, v/v). The determination was performed by high performance liquid chromatography coupled with ion trap mass spectrometry (HPLC-IT-MS) using a negative electrospray ionization interface in the multiple reaction monitoring (MRM) mode. The transitions of m/z 339 -> 167 for diphacinone and m/z 373 -> 201 for chlorophacinone were selected for the quantificantions. For the whole blood samples, the calibration curves were linear within the ranges of 1.0 - 200.0 mu g/L and 0.5 - 100.0 mu g/L; the limits of quantification were 1.0 mu g/L and 0.5 mu g/L; the spike recoveries were 90.1% - 92.2% and 87.6% - 93.4%, the intra-day relative standard deviations (RSDs) were less than 6.8% and 7.4%, and the inter-day RSDs were less than 9.9% and 10.9% for diphacinone and chlorophacinone, respectively. For the urine samples, the calibration curves were linear within the ranges of 0.2 - 40.0 mu g/L and 0.1 - 20.0 mu g/L, the limits of quantification were 0.2 mu g/L and 0.1 mu g/L; the spike recoveries were 90.1% - 94.5% and 90.0% - 98.0%, the intra-day RSDs were less than 6.1% and 7.3%, and the inter-day RSDs were less than 8.9% and 11.2% for diphacinone and chlorophacinone, respectively. This method is simple and sensitive for the satisfactory determination of trace diphacinone and chlorophacinone residues in poisoned patients for the clinical diagnosis.
英文关键词high performance liquid chromatography-ion trap mass spectrometry (HPLC-IT- MS) diphacinone chlorophacinone whole blood urine
类型Article
语种英语
收录类别ESCI
WOS记录号WOS:000435242000016
WOS类目Chemistry, Analytical
WOS研究方向Chemistry
资源类型期刊论文
条目标识符http://119.78.100.177/qdio/handle/2XILL650/329594
作者单位[Jin Micong; Chen Xiaohong] Ningbo Municipal Ctr Dis Control & Prevent, Ningbo Key Lab Poison Res & Control, Ningbo 315010, Zhejiang, Peoples R China
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Jin Micong,Chen Xiaohong. Simultaneous determination of trace diphacinone and chlorophacinone in biological samples by high performance liquid chromatography coupled with ion trap mass spectrometry[J],2010,28(2):197-203.
APA Jin Micong,&Chen Xiaohong.(2010).Simultaneous determination of trace diphacinone and chlorophacinone in biological samples by high performance liquid chromatography coupled with ion trap mass spectrometry.CHINESE JOURNAL OF CHROMATOGRAPHY,28(2),197-203.
MLA Jin Micong,et al."Simultaneous determination of trace diphacinone and chlorophacinone in biological samples by high performance liquid chromatography coupled with ion trap mass spectrometry".CHINESE JOURNAL OF CHROMATOGRAPHY 28.2(2010):197-203.
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