Xiao Yongjun, Wong Wen Yee, Chan Li Yan, Yong Chee Keat, Abe Kosuke, Hancock Peter, Hird Simon
International Food & Water Research Centre, Waters Pacific Pte Ltd., 1 Science Park Road #01-10, The Capricorn, Singapore Science Park II, Singapore 117528, Singapore.
Nisshin Global Research Center Sdn. Bhd., Lot. 1, Lebuh Sultan Hishamudin 2, Kawasan 20, Bandar Sultan Suleiman, Port Klang 42009, Selangor, Malaysia.
Toxics. 2023 Feb 21;11(3):200. doi: 10.3390/toxics11030200.
Although the use of phthalates has been restricted worldwide, they remain an issue due to health concerns. Diet is one of the most important exposure pathways for humans and due to their solubility in oil, phthalates are commonly found in edible oil and food high in fat. Gas chromatography-mass spectrometry (GC-MS) using electron ionization (EI) has been commonly used for the analysis of the phthalates in foodstuffs, including edible oil. However, this method suffers from issues with sensitivity and selectivity, as most phthalates are fragmented to generate a common phthalic anhydride fragment ion at 149. The molecular ion cannot be observed due to strong fragmentation in EI. In contrast, atmospheric pressure gas chromatography (APGC) is a soft ionization technique with less fragmentation, whereby the molecular ion can be used as the precursor ion for multiple reaction monitoring (MRM). In this study, a simple and quick method for the determination of phthalates in vegetable oil using APGC-MS/MS was developed, and performance was assessed. The method was based on dilution of the oil in solvent and direct injection without the need for further cleanup. The established method was evaluated for linearity, recovery, precision, method detection limit (MDL), and method quantitation limit (MQL). The obtained MQL in vegetable oil was in the range of 0.015-0.058 mg/kg, despite limiting the injection volume to 1 µL, which is suitable for investigating dietary exposure and future proof against decreases to the regulatory limit. Finally, the developed method was successfully applied to analyze nine phthalates in eight commercially available vegetable oil.
尽管邻苯二甲酸盐的使用在全球范围内已受到限制,但出于对健康的担忧,它们仍然是一个问题。饮食是人类最重要的接触途径之一,由于邻苯二甲酸盐可溶于油,因此在食用油和高脂肪食物中普遍存在。使用电子电离(EI)的气相色谱-质谱联用(GC-MS)已常用于分析食品(包括食用油)中的邻苯二甲酸盐。然而,该方法存在灵敏度和选择性方面的问题,因为大多数邻苯二甲酸盐会发生碎片化,在质荷比为149处产生常见的邻苯二甲酸酐碎片离子。由于在EI中强烈的碎片化,无法观察到分子离子。相比之下,大气压气相色谱(APGC)是一种碎片化较少的软电离技术,分子离子可作为多反应监测(MRM)的前体离子。在本研究中,开发了一种使用APGC-MS/MS测定植物油中邻苯二甲酸盐的简单快速方法,并对其性能进行了评估。该方法基于将油稀释在溶剂中并直接进样,无需进一步净化。对建立的方法进行了线性、回收率、精密度、方法检出限(MDL)和方法定量限(MQL)评估。尽管将进样体积限制为1μL,但在植物油中获得的MQL范围为0.015-0.058mg/kg,这适用于调查膳食暴露情况,并能应对未来监管限值降低的情况。最后将所开发的方法成功应用于分析八种市售植物油中的九种邻苯二甲酸盐。