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| 低温法检测菜籽油黄曲霉毒素B1的研究 |
| Determination of aflatoxin B1 in rapeseed oil by low temperature method |
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| DOI：10.12166/j.zgyz.1003-7969/2020.01.011 |
| 中文关键词: 菜籽油 黄曲霉毒素B1 低温 检测 高效液相色谱 |
| 英文关键词:rapeseed oil aflatoxin B1 low temperature detection HPLC |
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| 中文摘要: |
| 按照GB 5009.22—2016《食品安全国家标准 食品中黄曲霉毒素B族和G族的测定》第二法检测菜籽油中黄曲霉毒素B1时存在杂峰较多、无法准确定性及定量等问题，本法在GB 5009.22—2016第二法的基础上优化了萃取溶剂，并通过降低萃取溶剂温度来降低菜籽油中杂质溶解度的方法，达到了理想的净化效果。在样品中加入已放入4 ℃冰箱冷藏30 min的甲醇-乙腈（体积比70∶ 30），振荡后取上清液氮吹至近干并衍生，衍生液氮吹至近干后利用初始流动相溶解并注入高效液相色谱仪检测。采用Waters XBridge BEH C18色谱柱（4.6 mm×100 mm, 2.5 μm），以蒸馏水和乙腈为流动相进行梯度洗脱，在流速0.8 mL/min、柱温40 ℃、进样量10 μL条件下，进行定性和定量分析。结果表明：方法线性范围为0.1～4.0 ng/mL，定量限为0.1 μg/kg,回收率为78.0%~90.4%，相对标准偏差为161%~4.15%。与国标方法相比，本方法可有效去除菜籽油中杂质，能准确地进行定性和定量，回收率和准确度均较好，可应用于菜籽油中黄曲霉毒素B1的日常检测。 |
| 英文摘要: |
| According to the GB 5009.22—2016 National Food Safety Standard for the Determination of Aflatoxin B and G in Foods, the second method for detecting aflatoxin B1 in rapeseed oil has many problems in getting miscellaneous peaks, uncertainty and quantification. The method optimized the extraction reagent based on the second method of GB 5009.22—2016, and reduced the solubility of the impurities in the rapeseed oil by reducing the temperature of the extractant to achieve an ideal purification effect.Methanol-acetonitrile (volume ratio 70∶ 30) placed in a refrigerator at 4 ℃ for 30 min was added to the sample. After shaking, the supernate was blown to near dryness and then derivatized, and then dissolved with initial mobile phase and injected to high performance liquid chromatography for detection. A Waters XBridge BEH C18 column (4.6 mm × 100 mm, 2.5 μm) was used with a gradient elution of distilled water and acetonitrile as the mobile phase. The flow rate was 0.8 mL/min, the column temperature was 40 ℃, and the injection volume was 10 μL for qualitative and quantitative analysis. Under the optimal conditions, the quantitative linear range,the limit of quantification, the recovery rate and the precision of the method were 0.1-4.0 ng/mL, 0.1 μg/kg, 78.0%-90.4% and 1.61%-4.15% respectively. Compared with the national standard, the method could effectively remove impurities from the rapeseed oil, accurately conduct qualitative and quantitative analysis, and had good recovery rate and accuracy, and could be applied to the daily detection of aflatoxin B1 in rapeseed oil. |
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