食品科学 ›› 2021, Vol. 42 ›› Issue (10): 322-329.doi: 10.7506/spkx1002-6630-20200416-207

• 安全检测 • 上一篇    

通过式SPE-UPLC-MS/MS测定植物油中的9 种酚类抗氧化剂

张艳侠,赵慧男,孙珊珊,徐向军,郑文静,薛霞,王明栋,刘艳明,祝建华   

  1. (1.山东省食品药品检验研究院,山东省特殊医学用途配方食品质量控制工程技术研究中心,山东省食品药品安全检测工程技术研究中心,山东 济南 250101;2.中国石化天然气分公司榆济管道公司,山东 济南 250101)
  • 出版日期:2021-05-25 发布日期:2021-06-02
  • 基金资助:
    山东省重点研发计划(医用食品专项计划)项目(2019YYSP020); “十三五”国家重点研发计划重点专项(2017YEC1601600)

Simultaneous Determination of Nine Phenolic Antioxidants in Vegetable Oil by Pass-through Solid Phase Extraction Cleanup and Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

ZHANG Yanxia, ZHAO Huinan, SUN Shanshan, XU Xiangjun, ZHENG Wenjing, XUE Xia, WANG Mingdong, LIU Yanming, ZHU Jianhua   

  1. (1. Shandong Research Center of Engineering and Technology for Quality Control of Food for Special Medical Purposes, Shandong Research Center of Engineering and Technology for Safety Inspection of Food and Drug, Shandong Institute for Food and Drug Control, Jinan 250101, China;2. Yulin-Jinan Gas Pipeline Division of Nature Gas Company, SINOPEC Tianranqi Company, Jinan 250101, China)
  • Online:2021-05-25 Published:2021-06-02

摘要: 建立采用通过式固相萃取柱净化,超高效液相色谱-串联质谱法同时检测植物油中9 种酚类抗氧化剂的方法。油样品中酚类抗氧化剂用酸化乙腈提取,正己烷除脂,上清液经Oasis? PRIME HLB通过式固相萃取柱净化,C18色谱柱分离,采用乙腈-水流动相进行梯度洗脱,三重四极杆质谱电喷雾多反应监测模式检测,外标法定量。结果表明:采用本实验建立的方法,没食子酸丙酯、2,4,5-三羟基苯丁酮、叔丁基对苯二酚、去甲二氢愈创木酸、叔丁基对羟基茴香醚、2,6-二叔丁基-4-羟甲基苯酚、没食子酸辛酯、2,6-二叔丁基对甲基苯酚及没食子酸十二酯9 种抗氧化剂在各自质量浓度范围内线性关系良好,相关系数(R2)大于0.994。其中9 种抗氧化剂的方法检出限(RSN=3)在0.003~0.02 mg/kg范围,定量限(RSN=10)在0.01~0.05 mg/kg范围。在0.05、5.0、50.0 mg/kg三个添加水平下,9 种抗氧化剂平均加标回收率在82.2%~115.2%之间,相对标准偏差均小于9.3%。该方法简单、高效、灵敏度高,适用于植物油中抗氧化剂的快速定性、定量分析。

关键词: 植物油;抗氧化剂;通过式固相萃取;超高效液相色谱-串联质谱法

Abstract: A method for the determination of nine phenolic antioxidants in vegetable oil by pass-through solid phase extraction (SPE) cleanup combined with ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was established. The antioxidants in samples were extracted with 0.5% formic acid-acetonitrile (V/V), purified by a pass-through SPE procedure on an Oasis? PRiME HLB column. The chromatographic separation was carried out using a C18 column with gradient elution using a mobile phase consisting of acetonitrile and water. The target compounds were detected by triple quadrupole mass spectrometry with electrospray ionization (ESI) under the multiple reaction monitoring (MRM) mode. The calibration curves of the nine antioxidants showed good linearity in their own ranges with correlation coefficients of higher than 0.994. The average recoveries ranged from 82.2% to 115.2% at three spiking levels with relative standard deviation (RSD) of less than 9.3%. The limits of detection (LODs) of the analytes were in the range of 0.003-0.02 mg/kg. The limits of quantitation (LOQs) of the analytes were in the range of 0.01–0.05 mg/kg. This rapid and sensitive method is suitable for the detection of antioxidants in vegetable oil.

Key words: vegetable oil; antioxidants; pass-through solid phase extraction cleanup; ultra-high performance liquid chromatography-tandem mass spectrometry

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