[Online gel permeation chromatography-gas chromatography-triple quadrupole mass spectrometry for determination of 18 polychlorinated biphenyls in serum].

Abstract

OBJECTIVE: To establish a rapid method for detecting 18 polychlorinated biphenyls（PCBs） in serum using online gel permeation chromatographygas chromatography-triple quadrupole mass spectrometry（GPC-GC-MS/MS）. METHODS: Isotopic internal standards were added to 100 μL serum samples. Following extraction with acetone-cyclohexane（3 ∶7,V/V） and dehydration with anhydrous sodium sulphate, the supernatant was concentrated and analysed by GPC-GC-MS/MS. Target compounds were separated using a DB-5MS column（30 m × 0.25 mm, 0.25 μm） for target compound separation. Detection employed multiple reaction monitoring mode with quantification via internal standardisation. RESULTS: The 18 PCBs exhibited good linearity within the concentration range of 0.01-5 ng/mL, with correlation coefficients（R2） all exceeding 0.997.The method limits of detection（LOD） ranged from 0.001 to 0.004 ng/mL. Spiked recovery rates for the 18 PCBs ranged from 80.9% to 118.6% at spiking levels of 0.01, 0.1 and 1ng/mL, with relative standard deviations（RSD） of 1.5% to 12.6%（n=6）. Comparing the result with those of human serum standard reference material SRM1958（0.00778-0.473 ng/g） showed that the coefficient of RSD was less than 10% for all 18 PCBs relative to the reference values. This indicates good accuracy and specificity. Application of the established method to 20 human serum samples from a specific region detected all 12 remaining PCBs, with the exception of PCB-81, PCB-77, PCB-123, PCB-114, PCB-126, and PCB-169.Detection rates ranged from 5% to 100%, with detection levels ranging from below the LOD to 0.807 2 ng/mL. CONCLUSION: This method demonstrates high precision and accuracy and provides an effective analytical approach for the rapid and sensitive detection of trace polychlorinated biphenyls in serum.

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