PMID- 20556961
OWN - NLM
STAT- MEDLINE
DCOM- 20120105
LR  - 20190923
IS  - 1000-8713 (Print)
IS  - 1000-8713 (Linking)
VI  - 28
IP  - 2
DP  - 2010 Feb
TI  - [Simultaneous determination of trace diphacinone and chlorophacinone in 
      biological samples by high performance liquid chromatography coupled with ion 
      trap mass spectrometry].
PG  - 197-203
AB  - 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 microm) 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 
      microg/L and 0.5 - 100.0 microg/L; the limits of quantification were 1.0 microg/L 
      and 0.5 microg/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 microg/L and 0.1 - 20.0 microg/L; the 
      limits of quantification were 0.2 microg/L and 0.1 microg/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.
FAU - Jin, Micong
AU  - Jin M
AD  - Ningbo Key Laboratory of Poison Research and Control, Ningbo Municipal Center for 
      Disease Control and Prevention, Ningbo 315010, China. jmcjc@163.com
FAU - Chen, Xiaohong
AU  - Chen X
LA  - chi
PT  - English Abstract
PT  - Journal Article
PT  - Research Support, Non-U.S. Gov't
PL  - China
TA  - Se Pu
JT  - Se pu = Chinese journal of chromatography
JID - 9424804
RN  - 0 (Indans)
RN  - 34Y6E0063Y (chlorophacinone)
RN  - 54CA01C6JX (diphenadione)
RN  - 5M7Y6274ZE (Phenindione)
SB  - IM
MH  - Chromatography, High Pressure Liquid/*methods
MH  - Humans
MH  - Indans/*blood/urine
MH  - Phenindione/*analogs & derivatives/blood/urine
MH  - Sensitivity and Specificity
MH  - Spectrometry, Mass, Electrospray Ionization/*methods
EDAT- 2010/06/19 06:00
MHDA- 2012/01/06 06:00
CRDT- 2010/06/19 06:00
PHST- 2010/06/19 06:00 [entrez]
PHST- 2010/06/19 06:00 [pubmed]
PHST- 2012/01/06 06:00 [medline]
AID - 10.3724/sp.j.1123.2012.00197 [doi]
PST - ppublish
SO  - Se Pu. 2010 Feb;28(2):197-203. doi: 10.3724/sp.j.1123.2012.00197.