首页|食用植物油中4种合成抗氧化剂的QuEChERS预处理技术研究

食用植物油中4种合成抗氧化剂的QuEChERS预处理技术研究

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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 mLα-硫辛酸作为保护剂)振荡提取1min,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。
QuEChERS pre-processing technology for detecting four synthetic antioxidants in edible vegetable oil
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 0.80%-4.97%.The average oil residue rate in the final extract solution of antioxidants was 0.006 1 g/mL,with a RSD of 4.81%.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.

QuEChERShigh performance liquid chromatographysynthetic antioxidantedible vegetable oil

朱蕊、薛斌、任兴发

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上海维乐希检测技术有限公司,上海 201613

月旭科技(上海)股份有限公司,上海 201613

上海理工大学上海食品快速检测工程技术研究中心,上海 200093

QuEChERS 高效液相色谱 合成抗氧化剂 食用植物油

2024

中国油脂
国家粮食储备局西安油脂科学研究设计院

中国油脂

CSTPCD北大核心
影响因子:0.842
ISSN:1003-7969
年,卷(期):2024.49(12)