| 朱洪亮1，倪炜华1，陈妍1，王丽丽1，陈召桂2,3.GPC-UPLC-MS/MS测定食用植物油中
交链孢霉毒素含量[J].中国油脂,2026,52(3):.[ZHU Hongliang1,NI Weihua1,CHEN Yan1,WANG Lili1,CHEN Zhaogui2,3.Determination of Alternaria toxins in edible vegetable oils by GPC-UPLC-MS/MS[J].China Oils and Fats,2026,52(3):.] |
| GPC-UPLC-MS/MS测定食用植物油中
交链孢霉毒素含量 |
| Determination of Alternaria toxins in edible vegetable oils by GPC-UPLC-MS/MS |
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投稿时间：2025-03-28 修订日期：2025-12-01 录用日期：2025-04-15
出版日期：2026-03-20
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| DOI：10.19902/j.cnki.zgyz.1003-7969.250163 |
| 中文关键词: 凝胶渗透色谱 超高效液相色谱-串联质谱法 食用植物油 交链孢霉毒素 |
| 英文关键词:GPC UPLC-MS/MS edible vegetable oil Alternaria toxins |
| 基金项目:嘉兴市科技计划项目(2023AY11009) |
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| Author Name | Affiliation | | ZHU Hongliang1,NI Weihua1,CHEN Yan1,WANG Lili1,CHEN Zhaogui2,3 | 1.Jiaxing Institute for Food, Drug and Product Quality Inspection and Testing, Jiaxing 314000,
Zhejiang, China
2.School of Food Science and Technology, Jiangnan University, Wuxi 214122,
Jiangsu, China
3.Zhejiang Wufangzhai Industrial Co. , Ltd. , Jiaxing 314000, Zhejiang, China |
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| 中文摘要: |
| 旨在监测食用植物油中交链孢霉毒素的污染水平，建立了一种采用凝胶渗透色谱（GPC）净化，超高效液相色谱-串联质谱(UPLC-MS/MS)法同时检测食用植物油中7种交链孢霉毒素含量的方法。样品用乙酸乙酯-环己烷（体积比1∶ 1）溶解后过GPC净化，收集1 200~1 920 s的净化液，采用Intersil ODS-3 C18色谱柱分离，用不同体积比的0.002%氨水-乙腈进行梯度洗脱，以电喷雾离子源负离子模式电离、多反应监测模式监测，外标法定量。结果表明：7种交链孢霉毒素在0.2～100.0 μg/L质量浓度范围内线性关系良好，相关系数大于0.998，检出限在0.21～0.49 μg/kg之间，定量限在0.70~1.66 μg/kg之间，加标回收率为81.00%～97.50%，6次重复测定值的相对标准偏差为2.59%～8.12%；基质效应不明显。综上，该方法操作快速、简单、准确度高，适用于食用植物油中交链孢霉毒素含量的测定。 |
| 英文摘要: |
| In order to monitor the contamination levels of Alternaria toxins in edible vegetable oils, a method was established for simultaneous determination of seven Alternaria toxins using GPC cleanup followed by ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). The edible vegetable oils were dissolved in ethyl acetate-cyclohexane (volume ratio 1∶ 1) and purified by GPC, with the eluent collected between 1 200 s and 1 920 s. Separation was achieved on an Intersil ODS-3 C18 column with gradient elution using 0.002% ammonia water-acetonitrile at varying ratios. Detection was performed in negative electrospray ionization mode with multiple reaction monitoring, and quantification was carried out using external standard calibration.The results showed that there was a good linear relationship (r>0.998) of the seven Alternaria toxins within the linear range of 0.2-100.0 μg/L. Method detection limits ranged from 0.21 μg/kg to 0.49 μg/kg, quantitative limit ranged from 0.70 μg/kg to 1.66 μg/kg, and the spiked recoveries were between 81.00% and 97.50%.The relative standard deviations for six replicate measurements ranged from 2.59% to 8.12%. The matrix effect was not significant. In conclusion, the method is rapid, simple, accurate, and suitable for the determination of Alternaria toxins in edible vegetable oils. |
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