Determination of Ultratrace Indicator Polychlorinated Biphenyls in Animal Feed by Gas Chromatography-Triple Quadrupole Mass Spectrometry with Isotope Internal Standards

1.
Institute of Quality Standards and Testing Technology for Agricultural Products, Chinese Academy of Agricultural Science, Key Laboratory of Agrifood Safety and Quality, Ministry of Agriculture, Beijing 10081, China;
2.
Liaoning Provincial Veterinary Medicine Feed Animal Product Quality and Safety Testing Center, Shenyang 110016, China

Received Date: 8 August 2018
Revised Date: 25 August 2018

Fund Project: This work was supported by the National Key R&D Program of China (No. 2017YFC1600300), the Shanghai Agriculture Applied Technology Development Program, China (No. 20160301) and the Chinese Academy of Agricultural Science Basal Research Fund (No. 1610072018006).

A method was developed for determination of 6 kinds of indictor polychlorinated biphenyls in animal feed by chromatography-tandem mass spectrometry (GC-MS/MS). Analytical procedure consisted of accelerate solvent extraction (ASE), lipid removal with 44% acidic silica and clean-up using a column packed with multilayer silica. The analytes were separated on a DB-5MS capillary column, detected with electron ionization (EI) and multiple reaction monitor mode (MRM), and quantified using isotope dilution technique. The result showed that the calibration curves with good correlation coefficients (R²>0.999) were obtained in the concentration range of 0.1-500.0 ng/mL. The average relative response factors of PCBs in calibration solvent were 1.08-1.21, and the limit of quantification were 5.5-9.2 pg/g. The average recoveries of PCBs in animal feed at two spiked concentration levels ranged from 92.8% to 109.7% with relative standard deviations (RSDs) of 1.6%-14.8% (n=5), and the average recoveries of quantitative internal standards were 32.6%-90.2%. Then the proposed method was successfully applied to detect the compound feed samples from the surrounding area of Beijing, and it was found that the 6 kinds of indictor PCBs were detected in all samples (n=10) with the total concentration ranges of 54.7-191.7 pg/g, which were far below the limit standard (10 μg/kg) of Chinese National Standards.

Determination of Ultratrace Indicator Polychlorinated Biphenyls in Animal Feed by Gas Chromatography-Triple Quadrupole Mass Spectrometry with Isotope Internal Standards

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