Citation: SUN Xin, QI Li, QIN Tingting, WANG Minglin. Determination of 19 phthalate esters in cucumbers using QuEChERS coupled with gas chromatography-triple quadrupole mass spectrometry[J]. Chinese Journal of Chromatography, ;2014, 32(11): 1260-1265. doi: 10.3724/SP.J.1123.2014.05004 shu

Determination of 19 phthalate esters in cucumbers using QuEChERS coupled with gas chromatography-triple quadrupole mass spectrometry

SUN Xin ¹ ,
QI Li ² ,
QIN Tingting ¹ ,
WANG Minglin ^1,,

1.
1. College of Food Science and Engineering, Shandong Agricultural University, Taian 271018, China;

Corresponding author: WANG Minglin,
Received Date: 7 May 2014
Available Online: 22 July 2014
Fund Project: 国家"十二五"科技支撑计划项目(2012BAK17B05) (2012BAK17B05)山东省发改委项目(编号2011-黄-19) (编号2011-黄-19)中国科学院活体分析化学重点实验室开放基金课题(ACL201306). (ACL201306)

An efficient method using QuEChERS equipped with triple quadrupole GC-MS/MS for the simultaneous detection of 19 phthalate acid ester residues in cucumbers was established. The phthalate acid esters were extracted from cucumber samples by ultrasonic with acetonitrile. The extracts were salted out and centrifuged with anhydrous magnesium sulfate and sodium chloride. The supernatants were enriched by vacuum distillation, and then purified by C18 adsorbent. The 19 phthalate esters were separated on an HP-5ms UI column (30 m×0.25 mm×0.25 μm), and determined using MS/MS in multiple reactions monitoring mode. The method showed favorable qualitative and quantitative analysis of the phthalate esters with good linearity (r ≥ 0.9995) in the linear range of 10-5000 μg/kg and the limits of detection (LODs) were 0.2-3.5 μg/kg. With the proposed method, the recoveries were evaluated in cucumbers at the spiked levels of 10, 100 and 500 μg/kg. The results showed that the average recoveries were ranged from 63.3%-127.8% and the relative standard deviations (RSDs) were 0.5%-13.3%. In short, the proposed method with high sensitivity and good accuracy can meet the determination requirements for multi-residues. Furthermore, the method can be applied for the simultaneous determination of phthalate acid esters in cucumbers.
- QuEChERS,
- gas chromatography-triple quadrupole mass spectrometry/mass spectrometry (GC-MS/MS),
- phthalate acid esters,
- cucumbers
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