QuEChERS-超高效液相色谱-串联质谱法 测定酥油中17种真菌毒素Determination of 17 mycotoxins in ghee by QuEChERS-ultra-high performance liquid chromatography-tandem mass spectrometry
旨在为酥油中真菌毒素污染风险的监测与防控提供技术支撑，建立了QuEChERS技术结合超高效液相色谱-串联质谱法（UPLC-MS/MS）测定酥油中17种真菌毒素的检测方法。酥油样品经过3%甲酸水和3%甲酸乙腈溶液分步提取后，加入MgSO4和NaCl进行盐析处理，通过0 ℃低温离心和正己烷除脂，以N-丙基乙二胺（PSA）和十八烷基键合硅胶（C18）吸附剂作为净化填料净化后，经ACQUITY UPLC BEH C18色谱柱（100 mm × 2.1 mm，1.7 μm）实现分离，采用多反应监测（MRM）模式检测，基质匹配曲线外标法定量。结果表明：17种真菌毒素在相应质量浓度范围内呈良好的线性关系，决...
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| Format: | Article |
| Language: | English |
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中粮工科（西安）国际工程有限公司
2025-07-01
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| Series: | Zhongguo youzhi |
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| Online Access: | http://tg.chinaoils.cn/zgyz/ch/reader/create_pdf.aspx?file_no=20250720&flag=1 |
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| Summary: | 旨在为酥油中真菌毒素污染风险的监测与防控提供技术支撑，建立了QuEChERS技术结合超高效液相色谱-串联质谱法（UPLC-MS/MS）测定酥油中17种真菌毒素的检测方法。酥油样品经过3%甲酸水和3%甲酸乙腈溶液分步提取后，加入MgSO4和NaCl进行盐析处理，通过0 ℃低温离心和正己烷除脂，以N-丙基乙二胺（PSA）和十八烷基键合硅胶（C18）吸附剂作为净化填料净化后，经ACQUITY UPLC BEH C18色谱柱（100 mm × 2.1 mm，1.7 μm）实现分离，采用多反应监测（MRM）模式检测，基质匹配曲线外标法定量。结果表明：17种真菌毒素在相应质量浓度范围内呈良好的线性关系，决定系数（R2）均大于0.999 1，该方法的检出限（LOD）为0.15~3.00 μg/kg，定量限（LOQ）为0.50~10.00 μg/kg；在1、2、10倍LOQ加标水平下，17种真菌毒素的回收率为723%~112.2%，相对标准偏差（RSD）均不大于8.0%；应用该方法对20批次酥油样品进行检测，在3批次样品中检出了伏马毒素B2，2批次样品中检出T-2毒素。综上，该方法具有灵敏度好，准确度高的特点，可作为酥油中真菌毒素的日常监测方法。
In order to provide technical support for the monitoring, prevention and control of the risk of mycotoxin contamination in ghee, a method for the determination of 17 mycotoxins in ghee by QuEChERS technique combined with ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed. The ghee sample was extracted with 3% formic acid in water and 3% formic acid in acetonitrile in a stepwise manner, and then salted with MgSO4 and NaCl. After centrifugation at 0 ℃ and defatting with n-hexane, the extract was purified with N-propylethylenediamine (PSA) and octadecylsilyl silica gel (C18) to obtain the test sample. The test sample was then analyzed on an ACQUITY UPLC BEH C18 (100 mm × 2.1 mm, 1.7 μm) column to achieve the separation, and detected in multiple reaction monitoring (MRM) mode and quantified by standard method with matrix matching curve external. The results showed that the 17 mycotoxins demonstrated good linearity in the corresponded mass concentration ranges with the coefficients of determination (R2) greater than 0.999 1. The limits of detection (LOD) and the limits of quantification (LOQ) of the method were in the range of 0.15-3.00 μg/kg and 0.50-10.00 μg/kg, respectively. The recoveries of the 17 mycotoxins ranged from 72.3% to 112.2% at 1, 2 and 10 times LOQ spiked levels with relative standard deviations (RSD) less than 8.0%. Twenty batches of ghee samples were analyzed and tested by this method, and fumonisin B2 was detected in three batches, while T-2 toxin was detected in two batches. In summary, the method is sensitive, accurate, and effective for routine monitoring of mycotoxins in ghee. |
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| ISSN: | 1003-7969 |