食品科学 ›› 2020, Vol. 41 ›› Issue (18): 275-282.doi: 10.7506/spkx1002-6630-20190721-269

• 安全检测 • 上一篇    下一篇

QuEChERS-同位素稀释-气相色谱-串联质谱同时测定植物油中16 种邻苯二甲酸酯

曾少甫,胡长鹰,冯志强   

  1. (1.广东省食品工业研究所有限公司,广东?广州 511442;2.广东省食品质量监督检验站,广东?广州 511442;3.暨南大学食品科学与工程系,广东?广州 510632)
  • 出版日期:2020-09-25 发布日期:2020-09-18
  • 基金资助:
    “十三五”国家重点研发计划重点专项(2018YFC1603205);广东省重点领域研发计划项目(2019B020212002)

Simultaneous Determination of 16 Phthalate Esters in Vegetable Oil by QuEChERS-Isotope Dilution-Gas Chromatography Mass Spectrometry

ZENG Shaofu, HU Changying, FENG Zhiqiang   

  1. (1. Guangdong Food Industry Institute Co. Ltd., Guangzhou 511442, China; 2. Guangdong Food Quality Supervision and Inspection Station, Guangzhou 511442, China; 3. Department of Food Science and Engineering, Jinan University, Guangzhou 510632, China)
  • Online:2020-09-25 Published:2020-09-18

摘要: 建立QuEChERS结合气相色谱-串联质谱法测定植物油中16?种邻苯二甲酸酯类的分析方法。以饱和正己烷的乙腈作为提取溶剂,无水硫酸镁为脱水剂。对提取时间、提取溶剂体积、净化剂品种选择和净化剂用量进行优化,并以玉米油、花生油和葵花籽油进行方法验证,同时对3?种植物油中邻苯二甲酸酯(phthalic acid esters,PAEs)检测的基质效应进行评估。气相色谱-质谱联用仪选择离子监测模式测定,基质内标法定量。结果表明,采用涡旋振荡提取,在提取时间2?min、提取溶剂体积4?mL时,提取效果最佳,经100?mg/mL十八烷基键合硅胶和50?mg/mL乙二胺-N-丙基硅烷的净化效果良好。16?种目标物在5~500?μg/L范围内线性良好,相关系数均大于0.999?0,方法的检出限和定量限分别为0.002~0.03?mg/kg和0.008~0.1?mg/kg,在3?个加标水平(0.04、0.2、0.4?mg/kg)的16?种PAEs在玉米油、花生油和葵花籽油基质的平均回收率在80.2%~118.6%之间,相对标准偏差为0.2%~9.8%。3?种植物油基质对PAEs均存在基质增强效应,其基质效应在11.0%~158.9%之间,采用基质匹配标准曲线法能改善基质效应的影响。该方法高效、简便、快速,可作为植物油中16?种PAEs的定性和定量检测手段。

关键词: QuEChERS;邻苯二甲酸酯;植物油;气相色谱-串联质谱;基质效应

Abstract: An analytical method for simultaneous determination of 16 phthalate esters (PAEs) s in vegetable oils by quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction combined with gas chromatography mass spectrometry (GC-MS) was established. Acetonitrile saturated with n-hexane was used as the extraction solvent and dehydrated with anhydrous magnesium sulfate. The extraction time, extraction solvent volume, and purifying agent type and dosage were optimized. The applicability of this analytical method was verified with corn oil, peanut oil and sunflower oil samples. Meanwhile, the matrix effect of PAEs detection in the three vegetable oils was also evaluated. The mass spectrometer was operated in the selected-ion monitoring (SIM) mode and the matrix-matched internal standard calibration method was used for quantification. Results showed that the best extraction efficiency was obtained after vortex oscillation for 2 min with 4 mL of the extraction solvent, and the best purification efficiency was achieved using 100 mg/mL octadecyl bonded silica gel (C18) and 50 mg/mL ethylenediamine-N-propylsilane (PSA). The calibration curves for all target analytes displayed good linear relationships over the concentration range of 5–500 μg/L, with correlations coefficients of more than 0.999 0. The limits of detection (LODs) and limits of quantitation (LOQs) were 0.002–0.03 mg/kg and 0.008–0.1 mg/kg respectively. The average recoveries of the 16 PAEs at three spiked levels (0.04, 0.2 and 0.4 mg/kg) from corn oil, peanut oil and sunflower oil ranged from 80.2% to 118.6%, with relative standard deviations (RSDs) of 0.2% to 9.8%. The 16 PAEs exhibited an enhanced matrix effect in the three oil matrices, with a percentage enhancement in the range of 11.0% to 158.9%. However, the matrix-matched curve was found to effectively eliminate the matrix effects. The method was efficient, simple rapid, and suitable for determining the residues of 16 PAEs in vegetable oils.

Key words: QuEChERS; phthalate esters; vegetable oil; gas chromatography-mass spectrometry; matrix effect

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