College of Food Engineering and Biotechnology, Tianjin Univ. of Science and Technology, Tianjin 300457, P. R. China.
Beijing Advanced Innovation Center for Food Nutrition and Human Health, Beijing Technology and Business Univ., Beijing 100048, P. R. China.
J Food Sci. 2018 Apr;83(4):892-901. doi: 10.1111/1750-3841.14063. Epub 2018 Mar 25.
A modified QuEChERS method coupled with gas chromatography-mass spectrometry (GC-MS) was developed for analysis of 14 phthalate esters (PAEs) in grain sorghum (GS). Chemical extraction was done with acetonitrile followed by dispersive-solid phase extraction technique with a mixture of sorbents including primary secondary amine and octadecyl silica. Under the optimized condition, the matrix-matched calibration curves for all PAEs showed good linear relationship in the concentration range between 5 and 500 μg/L with correlation coefficients (R ) better than 0.99. Mean recoveries were between 82.0% and 120.2% at spiking levels of 0.06, 0.6, and 2.0 mg/kg with RSD of 0.3% to 7.8% (n = 5) for intra-day precision and 1.2% to 7.6% (n = 5) for inter-day precision. The LOD and LOQ for 14 PAEs were between 0.4 and 10.0 μg/kg and 0.5 and 20.0 μg/kg, respectively. Analysis of 32 commercial GS samples revealed that dimethyl-, diethyl-, diisobutyl-, dibutyl-, and di- (2-ethylhexyl) phthalate esters were detected in all of the analytes. In addition, content-color scale model was applied to visualize the concentration differences of PAEs in real GS samples. Principal component analysis of PAEs revealed that the GS samples did not have a distinctive cluster based on their geographic origins. The established method was proven to be simple, accurate, and effective for analysis of PAEs in GS, which might also be applied for analysis of PAEs in other matrices.
A modified QuEChERS-based GC-MS method was developed for the determination of phthalate esters (PAEs) in grain sorghum (GS). The ubiquitous presence of PAEs can migrate into GS. Therefore, evaluation of the total content of PAEs in GS is helpful to understand its impact of overall pollution level on other foods. This study has provided some basic information in terms of the content and contamination of PAEs in GS, which is helpful to establish relevant standards and risk assessment of GS for the government.
本研究建立了一种改良的 QuEChERS 方法，结合气相色谱-质谱（GC-MS）分析高粱中的 14 种邻苯二甲酸酯（PAEs）。采用乙腈进行化学萃取，然后采用包括伯仲胺和十八烷基硅烷在内的混合吸附剂进行分散固相萃取技术。在优化条件下，所有 PAEs 的基质匹配校准曲线在 5 至 500μg/L 的浓度范围内均表现出良好的线性关系，相关系数（R）均大于 0.99。在 0.06、0.6 和 2.0mg/kg 的添加水平下，平均回收率在 82.0%至 120.2%之间，日内精密度的相对标准偏差（RSD）为 0.3%至 7.8%（n=5），日间精密度为 1.2%至 7.6%（n=5）。14 种 PAEs 的检出限和定量限分别为 0.4 至 10.0μg/kg 和 0.5 至 20.0μg/kg。对 32 个商业高粱样品的分析表明，所有分析物中均检测到二甲基、二乙基、二异丁基、二丁基和二（2-乙基己基）邻苯二甲酸酯。此外，还应用含量-颜色比例模型直观地显示了实际高粱样品中 PAEs 的浓度差异。PAEs 的主成分分析表明，根据地理来源，高粱样品没有明显的聚类。该方法被证明简单、准确、有效，可用于高粱中 PAEs 的分析，也可用于其他基质中 PAEs 的分析。
本研究建立了一种基于 QuEChERS 的 GC-MS 方法，用于测定高粱中的邻苯二甲酸酯（PAEs）。PAEs 的普遍存在可能会迁移到高粱中。因此，评估高粱中 PAEs 的总含量有助于了解其对其他食物整体污染水平的影响。本研究为高粱中 PAEs 的含量和污染情况提供了一些基本信息，有助于政府制定相关的高粱标准和风险评估。
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