Premium
Simultaneous detection of multiple hydroxylated polychlorinated biphenyls from biological samples using ultra‐high‐performance liquid chromatography with isotope dilution tandem mass spectrometry
Author(s) -
Zheng Yibin,
Cai Delei,
Huang Baifen,
Han Jianlong,
Chen Qing,
Zhang Jingshun,
Zhang Jie,
Wang Xiaofeng,
Shen Haitao
Publication year - 2019
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.201800831
Subject(s) - chromatography , chemistry , ammonium formate , isotope dilution , detection limit , tandem mass spectrometry , mass spectrometry , electrospray ionization , extraction (chemistry) , elution , high performance liquid chromatography , electrospray , solid phase extraction
We established a method for the separation and detection of nine hydroxylated polychlorinated biphenyls in whole blood and urine samples using ultra high performance liquid chromatography coupled with electrospray negative ionization tandem mass spectrometry. Clean‐up procedures involved a filtration step, and optimization involved a pretreatment step consisting of a simple liquid–liquid extraction using hydrated silica‐gel chromatography (5%). Nine hydroxylated polychlorinated biphenyls were separated on an ultra high performance liquid chromatography HSS T3 column using a gradient elution program of 2 mmol ammonium formate aqueous solution (A) and methanol (B). Recovery ranged from 84.0 to 105.4% for the nine different hydroxylated polychlorinated biphenyls in urine with three spiked levels of 0.1, 1, and 2 ng and from 73.5 to 98.6% for the blood with spiked levels of 0.2, 1, and 2 ng. The relative standard deviations were <8.7% ( n = 6), and the limits of detection in urine and whole blood for the nine hydroxylated polychlorinated biphenyls were in the range of 1.5–4 and 20–100 pg/g, respectively. This analytical method may enable the simultaneous detection of various hydroxylated polychlorinated biphenyls from complex tissue matrices.