QuEChERS-气相色谱-三重四极杆质谱法检测黄瓜中的19种邻苯二甲酸酯

Determination of 19 phthalate esters in cucumbers using QuEChERS coupled with gas chromatographytriple quadrupole mass spectrometry

建立了 QuEChERS 结合气相色谱-三重四极杆质谱联用仪同时检测黄瓜中19种邻苯二甲酸酯残留的方法。黄瓜样品采用乙腈超声提取，经无水硫酸镁和氯化钠盐析离心后减压蒸馏富集，然后用 C18吸附剂净化，经HP-5ms UI色谱柱分离后在多反应监测模式下进行测定。该方法在10-5000μg / kg 范围内线性关系良好（ r ≥0.9995），检出限为0.2-3.5μg / kg。按照建立的方法分别进行了10、100和500μg / kg 3个添加水平的19种邻苯二甲酸酯的加标回收率试验，回收率为63.3％-127.8％，相对标准偏差为0.5％-13.3％。该方法灵敏度高、准确度好，符合多残留检测的技术要求，适用于黄瓜等蔬菜中邻苯二甲酸酯残留的检测。

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 ad-sorbent. 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. 999 5）in the linear range of 10-5 000 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.