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| 固相萃取净化-超高效液相色谱串联质谱法测定菜籽油中交链孢霉毒素含量 |
| Determination of alternaria mycotoxins in rapeseed oil by solid phase extraction with ultra high performance liquid chromatography-tandem mass spectrometry |
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| DOI： |
| 中文关键词: 交链孢霉毒素 固相萃取 超高效液相色谱串联质谱法 菜籽油 |
| 英文关键词:alternaria mycotoxins solid phase extraction ultra high performance liquid chromatography-tandem mass spectrometry rapeseed oil |
| 基金项目: |
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| 中文摘要: |
| 建立了固相萃取净化-超高效液相色谱串联质谱法测定菜籽油中交链孢霉毒素含量的方法。将菜籽油与甲醇混匀后使用 Captive EMR-Lipid 固相萃取柱（3 mL, 300 mg）净化，收集净化液经氮吹浓缩后，采用超高效液相色谱串联质谱测定，内标法定量。以回收率为指标对固相萃取柱的净化载量及洗脱剂体积进行优化。结果表明，菜籽油最佳净化载量为0.15 g，最佳洗脱剂体积为2.0 mL。4种交链孢霉毒素在线性范围内相关系数均大于0.998，4种交链孢霉毒素加标回收率为688%~117.3%，精密度为8.6%~11.4%，方法检出限为0.1~2.0 μg/kg，定量限为0.3~6.0 μg/kg。方法具有较好的灵敏度及回收率，简单、易于操作，适用于菜籽油中交链孢霉毒素的检测。 |
| 英文摘要: |
| A method for analysis of alternaria mycotoxins in rapeseed oil was established by solid phase extraction with ultra high performance liquid chromatography- tandem mass spectrometry. The rapeseed oil was mixed with methanol and purified by Captive EMR-Lipid solid phase extraction column (3 mL, 300 mg). The purification liquid was collected and concentrated by nitrogen blowing. The alternaria mycotoxins were determined by ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) and quantified by internal standard method. The purification capacity and eluent volume were optimized by investigating the recovery rate of alternaria mycotoxins. The results showed that the optimal purification capacity of rapeseed oil was 0.15 g, and the optimal eluent volume was 2.0 mL. The correlation coefficients of alternaria mycotoxins within linear range were greater than 0.998, and the recovery rates of alternaria mycotoxins ranged from 68.8% to 117.3% with the relative standard deviations of 8.6%-11.4%. The limit of detection and limit of quantification were 0.1-2.0 μg/kg and 0.3-6.0 μg/kg, respectively. The method had good sensitivity and recovery rate, and it was simple and easy to operate. The method was suitable for determination of alternaria mycotoxins in rapeseed oil. |
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