HPTLC-DPPH显色-像素分析快速测定酚类抗氧化剂:以食用油和烘焙食品中TBHQ为例  

HPTLC-DPPH colorimetric-bioautographic image quantification of phenolic antioxidant: taking TBHQ in edible oil and baking foods as an example

作　　者：卫晓 席兴军[2] 李慧[3] 王小三[1] 黄丹菲[4] 徐学明[1] 陈启飞 黄晓倩 陈益胜 WEI Xiao;XI Xingjun;LI Hui;WANG Xiaosan;HUANG Danfei;XU Xueming;CHEN Qifei;HUANG Xiaoqian;CHEN Yisheng(School of Food Science and Technology,Jiangnan University,Wuxi 214122,Jiangsu,China;China National Institute of Standardization,Beijing 100191,China;Oil Crops Research Institute,Chinese Academy of Agricultural Sciences,Wuhan 430062,China;State Key Laboratory of Food Science and Technology,Nanchang University,Nanchang 330047,China)

机构地区：[1]江南大学食品学院,江苏无锡214122 [2]中国标准化研究院,北京100191 [3]中国农业科学院油料作物研究所,武汉430062 [4]南昌大学食品科学与技术国家重点实验室,南昌330047

出　　处：《中国油脂》2022年第3期105-109,127,共6页China Oils and Fats

基　　金：国家自然科学基金项目(21804058);南昌大学食品科学与技术国家重点实验室开放基金项目(SKLF-KF-202001)。

摘　　要：目前,酚类抗氧化剂TBHQ的常用检测方法存在前处理烦琐、耗时长、单次只能测定一个样品的问题,因此亟需建立一种高通量、快速准确的检测方法。为此,将高效薄层色谱(HPTLC)分离与1,1-二苯基-2-三硝基苯肼(DPPH)还原变色反应、图像像素定量分析相结合,建立了一种快速筛检酚类抗氧化剂TBHQ的方法。在此基础上,以食用油、面包和蛋糕为代表性样品,验证所建方法的实际应用性能。结果显示:所建方法检测TBHQ的检测限为70 ng/zone (35 mg/kg),定量限为140 ng/zone (70 mg/kg),定量限低于GB 2760—2014规定的使用限量(200 mg/kg);通过对比分析,样品提取物中共存的背景基质对目标物定量的干扰可以忽略,证明了该方法具有良好的选择性;目标物在150~550 ng/zone范围内表现出良好的线性(R^(2)=0.989 2);多次平行(n=3)测试和国标规定使用限量水平附近的加标回收率测试结果证明了该方法具有较好的精密度和准确度。综上,该方法具有基质耐受性强、定量准确、简便可靠且分析通量大等优点,特别适合粮油食品中各种抗氧化剂的快速定量筛查,具有凝炼成为相关领域国家标准的潜力和价值。At present, the common detection methods of phenolic antioxidant TBHQ have the problems of cumbersome pretreatment, long time-consuming and can only determine one sample at a time. Therefore, it is urgent to establish a high-throughput, fast and accurate detection method. A rapid method for screening phenolic antioxidant TBHQ was established by combining high performance thin layer chromatography(HPTLC) separation with reduction discoloration reaction of 1,1-diphenyl-2-trinitrophenylhydrazine(DPPH) and quantitative analysis of image pixels. On this basis, edible oil, bread and cake were taken as representative samples to verify the practical application performance of the proposed method. The results showed that the detection limit of the established method to detect TBHQ was 70 ng/zone(35 mg/kg), the limit of quantification was 140 ng/zone(70 mg/kg), and the limit of quantification was lower than the limit of use(200 mg/kg) specified in GB 2760-2014. Through comparative analysis, the interference of the background matrix coexisting in the sample extract on the target quantity could be ignored, which proved that the method had good selectivity. The target showed good linearity in the range of 150-550 ng/zone(R^(2)=0.989 2). Secondly, several parallel tests(n=3) and the test results of spiked recovery near the specified limit level of national standard proved that the method had good precision and accuracy. In summary, this method has the advantages of strong matrix tolerance, accurate quantification, simpleness and reliableness, and large analytical flux. Therefore, it is particularly suitable for rapid quantitative screening of various antioxidant additives in cereal and oil food, and has the potential and value of becoming a national standard in related fields.

关 键 词：HPTLC DPPH TBHQ 粮油食品 

分 类 号：TS207[轻工技术与工程—食品科学] O657[轻工技术与工程—食品科学与工程]