Citation: XU Juan, WANG Lan, HUANG Huajun, CHEN Jie, CHEN Wenrui, XIANG Dapeng. Low temperature freezing followed by dispersive solid phase extraction for the determination of 104 pesticide residues in vegetable oils using ultra-performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, ;2015, 33(3): 242-249. doi: 10.3724/SP.J.1123.2014.10011 shu

Low temperature freezing followed by dispersive solid phase extraction for the determination of 104 pesticide residues in vegetable oils using ultra-performance liquid chromatography-tandem mass spectrometry

1.
Guangdong Entry-Exit Inspection and Quarantine Bureau, Guangzhou 510623, China

Corresponding author: HUANG Huajun,
Received Date: 20 October 2014
Available Online: 22 December 2014
Fund Project: 广东检验检疫局科技计划项目(2012GDK36) (2012GDK36)国家质检总局公益性行业科研专项(201410177). (201410177)

A method using liquid-liquid extraction (LLE) followed by clean-up steps of centrifugation, freezing and dispersive solid phase extraction (D-SPE)and ultra-performance liquid chromatography (UPLC) coupled with tandem mass spectrometry (MS/MS) has been developed for the determination of trace levels of 104 pesticides in vegetable oils. LLE has been optimized to extract these pesticide residues from oils to obtain the highest recoveries of pesticides and the lowest co-extract fat residue in the final extract. In addition, the centrifugation and freezing steps as well as D-SPE with primary secondary amine (PSA), graphite carbon black (GCB) and C18 were used as the clean-up steps to minimize the co-extract fat. The recoveries obtained ranged from 55% to 121% and the relative standard deviations (RSDs) ranged from 0.47% to 19.2% at the spiked levels of 0.01, 0.02 and 0.05 mg/kg. This method, combining with accurate and sensitive detection, allowed quantification and confirmation at levels as low as 1 μg/kg for 80% of the analytes. The limits of quantification (LOQs) of the most compounds were below the maximum residue limits (MRLs) established by the Chinese legislations for oils. The proposed method was applied successfully for the residue determination of the selected pesticides in oils.
- liquid-liquid extraction (LLE),
- dispersive solid phase extraction (D-SPE),
- ultra-performance liquid chromatography (UPLC),
- tandem mass spectrometry (MS/MS),
- pesticides,
- vegetable oils,
- residues
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沈阳化工大学材料科学与工程学院沈阳 110142