PMID- 12530820
OWN - NLM
STAT- MEDLINE
DCOM- 20030429
LR  - 20191210
IS  - 0003-2700 (Print)
IS  - 0003-2700 (Linking)
VI  - 75
IP  - 1
DP  - 2003 Jan 1
TI  - Comprehensive solid-phase extraction method for persistent organic pollutants. 
      Validation and application to the analysis of persistent chlorinated pesticides.
PG  - 71-7
AB  - The Centers for Disease Control and Prevention (CDC) is involved in many 
      epidemiological studies regarding the measurement of chlorinated pesticides and 
      polychlorinated biphenyls in specimens obtained from humans. In addition to these 
      commonly determined analytes, there is a need to include additional persistent 
      organic pollutants (POPs) in our analyses, which further stresses the analyses 
      because sample volumes remain small. Thus, a single method of analysis for all 
      POPs in human serum is needed. CDC has recently developed a semiautomated and 
      comprehensive solid-phase extraction method for POPs. The method is comprehensive 
      since it was optimized for the extraction of many different POP compound classes. 
      We then developed a purification and fractionation scheme that allows (a) 
      separation of different compound classes by particular functionalities and (b) 
      purification of those fractions to remove coextracted interferences. This paper 
      describes the first step in the semiautomated comprehensive extraction and 
      multiple fractionation method developed by CDC for monitoring POPs. In this 
      paper, we validate the analysis of the persistent chlorinated pesticides, a 
      compound class difficult to examine because of their structural diversity, in 
      human plasma. The method was validated against an existing CDC method by using a 
      spiked quality-control serum pool. The concentrations determined for all analytes 
      using both methods were within 2%-14% relative standard deviations. A multilevel 
      (i.e., 3-4 point) matrix spike showed good linearity for the analytes tested (r2 
      = 0.978-0.999). The method was then applied to 40-year-old archived plasma 
      samples for the quantitative analysis of selected chlorinated pesticides. Mean 
      recoveries of the 13C-labeled internal quantification standards ranged from 64% 
      to 123% for the 11 monitored pesticides. The overall method proved to be robust 
      by handling old coagulated plasma samples. It allowed faster throughput of 
      samples than our previous methods and provided cleaner samples with less frequent 
      interferences or background as analyzed by high-resolution mass spectrometry. The 
      method represents a preliminary step in establishing an automated, comprehensive 
      multiresidue analysis method for POPs in human serum.
FAU - Sandau, Courtney D
AU  - Sandau CD
AD  - National Center for Environmental Health, Centers for Disease Control and 
      Prevention, 4770 Buford Highway NE, Mailstop F17, Atlanta, Georgia, 30341-3724, 
      USA. csandau@cdc.gov
FAU - Sjodin, Andreas
AU  - Sjodin A
FAU - Davis, Mark D
AU  - Davis MD
FAU - Barr, John R
AU  - Barr JR
FAU - Maggio, Vincent L
AU  - Maggio VL
FAU - Waterman, Alyson L
AU  - Waterman AL
FAU - Preston, Kerry E
AU  - Preston KE
FAU - Preau, James L Jr
AU  - Preau JL Jr
FAU - Barr, Dana B
AU  - Barr DB
FAU - Needham, Larry L
AU  - Needham LL
FAU - Patterson, Donald G Jr
AU  - Patterson DG Jr
LA  - eng
PT  - Journal Article
PL  - United States
TA  - Anal Chem
JT  - Analytical chemistry
JID - 0370536
RN  - 0 (Environmental Pollutants)
RN  - 0 (Pesticides)
SB  - IM
MH  - Automation
MH  - Blood Chemical Analysis/*methods
MH  - Centers for Disease Control and Prevention, U.S.
MH  - Environmental Pollutants/*analysis/*blood
MH  - Humans
MH  - Pesticides/*analysis/*blood/chemistry
MH  - Reproducibility of Results
MH  - Sensitivity and Specificity
MH  - United States
EDAT- 2003/01/18 04:00
MHDA- 2003/04/30 05:00
CRDT- 2003/01/18 04:00
PHST- 2003/01/18 04:00 [pubmed]
PHST- 2003/04/30 05:00 [medline]
PHST- 2003/01/18 04:00 [entrez]
AID - 10.1021/ac026121u [doi]
PST - ppublish
SO  - Anal Chem. 2003 Jan 1;75(1):71-7. doi: 10.1021/ac026121u.