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Title

Determination of polychlorinated biphenyls and organochlorine pesticides in small volumes of human blood by high-throughput on-line SPE-LVI-GC-HRMS

Summary A fully automated and robust method featuring on-line solid-phase extraction (SPE) and large volume injection (LVI) gas chromatographic (GC) high resolution mass spectrometry (HRMS) is used to determine polychlorinated biphenyls (PCBs) and organochlorine pesticides, such as penta- and hexachloroben- zene (PeCBz, HxCBz), hexachlorocyclohexane isomers (HCH) and 4,4* -dichlorodiphenyldichloroethene (a metabolite of dichlorodiphenyltrichloroethane (DDT)), with only 200 l of human blood, serum or plasma. After spiking the sample with 13 C-labeled internal standards and precipitating the proteins, the sample is passed through a 10 mm × 2.0 mm ID SPE cartridge ?lled with C18 material that adsorbs the analytes. After washing and drying, the cartridge is extracted with hexane/dodecane (99/1, v/v); the extract is directly injected into a LVI where GC/HRMS analysis follows. The fully automated system uti- lizes a robotic autosampler and a modular SPE system including two high-pressure syringe pumps, an automatic SPE cartridge exchanger unit and 6 switchable valves. All sample preparation steps are per- formed within 20 min during the GC run of a previous sample, limiting the throughput with only the GC runtime. The contents are quanti?ed using the isotope dilution method. Due to laboratory air contam- ination problems, we achieved LOQs of 0.017 (PeCBz), 0.009 (HxCBz), 0.007 (HCH), 0.016 (DDE), while for the six indicator PCBs, we achieved values of 0.030 (PCB-28), 0.044 (PCB-52), 0.024 (PCB-101), 0.009 (PCB-138), 0.015 (PCB-153) and 0.008 (PCB-180) g/l serum. Under clean laboratory air conditions, these values may be improved. This method is recommended when high throughput is desirable and/or only small amounts of material are available, such as during studies involving children.
Category 3. Symbiosis User Application
These are applications that have been made by Symbiosis customers. They are validated and have been published.
 
Matrix Human blood
Market Clinical
Cartridge HySphere C18 HD
Detection GC with LVI
Compounds HCH (alpha- beta-, gamma-) HCH (alpha- beta-, gamma-) HCH (alpha- beta-, gamma-) HCH (alpha- beta-, gamma-) PFK-LMS PFK-LM PeCBz PeCBz PeCBz PeCBz HxCBz HxCBz HxCBz HxCBz TrCB (28) TrCB (28) TrCB (28) TrCB (28) TeCB (52) TeCB (52) PFK-LMS PFK-LM TeCB (52) TeCB (52) TeCB (81, 77) TeCB (81, 77) PFK-LMS PFK-LM TeCB (81, 77) TeCB (81, 77) 4,4* -DDE 4,4* -DDE PeCB (101) PeCB (101) 4,4* -DDE 4,4* -DDE PeCB (101) PeCB (101) PeCB (123, 118, 114, 105, 126) PeCB (123, 118, 114, 105, 126) PeCB (123, 118, 114, 105, 126) PeCB (123, 118, 114, 105, 126) PFK-LMS PFK-LM HxCB (153, 138, 167, 156, 157) HxCB (153, 138, 167, 156, 157) HxCB (153, 138, 167, 156, 157) HxCB (153, 138, 167, 156, 157) HxCB (169) HxCB (169) HxCB (169) HxCB (169) PFK-LMS PFK-LM HpCB (180, 189) HpCB (180, 189) HpCB (180, 189) HpCB (180, 189)
Compound Group polychlorinated biphenyls and organochlorine pesticides
Sample_volume 500 µL
 
Contact Jürgen Wittsiepe , Marco Nestola , Matthias Kohne, Peter Zinn , Michael Wilhelm
Account Department of Hygiene, Social and Environmental Medicine, Ruhr-University Bochum, Universitätsstraße 150, D-44801 Bochum, Germany Instrumental Analytical Chemistry, University Duisburg-Essen, Universitätsstraße 5, D-45141 Essen, Germany Department of Analytical Chemistry, Ruhr-University Bochum, Universitätsstraße 150, D-44801 Bochum, Germany
Published J. Wittsiepe et al. / J. Chromatogr. B 945-946 (2014) 217-224
Date 4-8-2015
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