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| 食用植物油中4种合成抗氧化剂的QuEChERS
预处理技术研究 |
| QuEChERS pre-processing technology for detecting four synthetic antioxidants in edible vegetable oil |
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| DOI：10.19902/j.cnki.zgyz.1003-7969.230669 |
| 中文关键词: QuEChERS 高效液相色谱 合成抗氧化剂 食用植物油 |
| 英文关键词:QuEChERS high performance liquid chromatography synthetic antioxidant edible vegetable oil |
| 基金项目:上海市“科技创新行动计划”科学仪器和化学试剂项目(21142203200) |
| Author Name | Affiliation | | ZHU Rui1,2，XUE Bin1,2，REN Xingfa2,3 | （1.Shanghai Weilexi Testing Technology Co. , Ltd. ，Shanghai 201613，China； 2.Welch Materials(Shanghai),
Inc. , Shanghai 201613, China； 3.Shanghai Engineering Research Center of Food Rapid Detection,
University of Shanghai for Science and Technology, Shanghai 200093, China） |
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| 中文摘要: |
| 为提高食用植物油中合成抗氧化剂相关检测工作的效率、便捷性和安全性，采用QuEChERS预处理技术，建立了同时从食用植物油中快速、高效提取，分离和净化没食子酸丙酯（PG）、叔丁基对苯二酚（TBHQ）、叔丁基对羟基茴香醚（BHA）和 2,6-二叔丁基对甲酚（BHT） 4种合成抗氧化剂的样品预处理方法，以用于高效液相色谱的检测。样品先采用乙腈-乙酸乙酯溶液（体积比3∶ 7）溶解并加入合成抗氧化剂专用提取吸附剂中静置，再加入萃取液（添加0.02 g/100 mL α-硫辛酸作为保护剂）振荡提取1 min，离心后取上层混合提取液加入C18E净化吸附剂中振荡提取2 min净化，离心分离后取上清液用高效液相色谱（配备二极管阵列检测器）对4种合成抗氧化剂含量进行测定，同时对色谱上样液中的油脂残留率进行测定。结果表明：4种合成抗氧化剂在1.0~100.0 mg/L范围内线性关系良好，检出限均可达4.0 mg/kg。在10、30、200、300 mg/kg 4个不同加标水平的平均回收率为82.08%～102.99%，相对标准偏差(RSD)为0.80%～4.97%。抗氧化剂色谱上样液中的平均油脂残留率为0.006 1 g/mL，RSD为4.81%。综上，建立的QuEChERS预处理技术具有操作简便快速、预处理效率高、结果准确性好、净化效果好等特点，适合食用植物油中4种合成抗氧化剂含量的检测与分析。 |
| 英文摘要: |
| In order to improve the efficiency, convenience, and safety of the detection of synthetic antioxidants in edible vegetable oil, QuEChERS pre-processing technology was used to establish a sample pretreatment method for the rapid and efficient extraction, separation, and purification of four synthetic antioxidants from edible vegetable oil, namely propyl gallate (PG), tert-butyl hydroquinone (TBHQ), butyl hydroxyanisole (BHA), and butylated hydroxytoluene (BHT) for detection by high performance liquid chromatography. The sample was first dissolved in acetonitrile-ethyl acetate solution (volume ratio 3∶ 7) and added to a specialized extraction adsorbent for synthetic antioxidants. Then, the extraction solution(adding 0.02% α-lipoic acid as a protective agent) was added for 1 min of oscillation extraction. After centrifugation, the upper layer of extraction solution was added to the purification adsorbent of C18E for 2 min of oscillation. After centrifugation, the upper layer of clear liquid was taken and the content of four antioxidants was measured using a high performance liquid chromatography equipped with diode array detector. At the same time, the oil residue rate in the final extraction solution for chromatographic determination was measured. The results showed that the four antioxidants had a good linear relationship within the range of 1.0-100.0 mg/L, and the detection limits was 4.0 mg/kg. The spiked recovery rate at four different levels of 10, 30, 200 mg/kg and 300 mg/kg was 82.08%-102.99%, and the relative standard deviation (RSD) was 080%-4.97%. The average oil residue rate in the final extract solution of antioxidants was 0.006 1 g/mL, with a RSD of 481%. In conclusion, this QuEChERS pre-processing technology established has the characteristics of simple and fast operation, high pretreatment efficiency, good accuracy of results, and good purification effect, and is suitable for the detection and analysis of four synthetic antioxidants in edible vegetable oils. |
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