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中国精品科技期刊2020
冯寅洁, 周小清, 乔勇升, 冯成玉. 三种专用固相萃取柱-高效液相色谱法检测食品中苏丹红含量[J]. 食品工业科技, 2020, 41(5): 232-238. DOI: 10.13386/j.issn1002-0306.2020.05.038
引用本文: 冯寅洁, 周小清, 乔勇升, 冯成玉. 三种专用固相萃取柱-高效液相色谱法检测食品中苏丹红含量[J]. 食品工业科技, 2020, 41(5): 232-238. DOI: 10.13386/j.issn1002-0306.2020.05.038
FENG Yin-jie, ZHOU Xiao-qing, QIAO Yong-sheng, FENG Cheng-yu. Determination of Sudan Dyes Contents in Foods by Three Special Solid Phase Extraction Cartridges Coupled with High Performance Liquid Chromatography[J]. Science and Technology of Food Industry, 2020, 41(5): 232-238. DOI: 10.13386/j.issn1002-0306.2020.05.038
Citation: FENG Yin-jie, ZHOU Xiao-qing, QIAO Yong-sheng, FENG Cheng-yu. Determination of Sudan Dyes Contents in Foods by Three Special Solid Phase Extraction Cartridges Coupled with High Performance Liquid Chromatography[J]. Science and Technology of Food Industry, 2020, 41(5): 232-238. DOI: 10.13386/j.issn1002-0306.2020.05.038

三种专用固相萃取柱-高效液相色谱法检测食品中苏丹红含量

Determination of Sudan Dyes Contents in Foods by Three Special Solid Phase Extraction Cartridges Coupled with High Performance Liquid Chromatography

  • 摘要: 建立了专用固相萃取柱-高效液相色谱法检测食品中苏丹红Ⅰ、Ⅱ、Ⅲ、Ⅳ的方法。样品经过正己烷提取,通过苏丹红专用固相萃取柱净化和富集,40℃水浴旋蒸至干后用甲基叔丁基醚-甲醇(体积比4:6)溶解定容,借助Waters Symmetry C18色谱柱(150 mm×4.6 mm,5 μm)分离,以乙腈-水为流动相梯度洗脱,二极管阵列检测器检测,外标法定量。结果表明,四种苏丹红在0.16~2.56 μg/mL内线性相关系数(r)均大于0.9999,不同食品的检出限在2.3~9.7 mg/kg之间。不同品牌的苏丹红专用固相萃取柱去除基质干扰和富集目标物的能力不同,可根据食品种类选择合适的固相萃取柱。ProElut SDH SPE柱普遍适用于不同种类食品的前处理;CNW Poly-sery MIP-SDR SPE柱适用于除辣椒粉以外的大部分食品的前处理;Cleanert Sudan SPE柱适用于浅色、低油脂食品的前处理。对六种食品加标2.0 mg/kg,经过ProElut SDH SPE柱处理后,回收率为83.7%~91.1%,相对标准偏差为2.4%~6.2%(n=6)。该方法净化和富集效果理想,与GB/T 19681-2005相比,具有操作简便、重复性好、准确度高、分析时间短、节省溶剂等特点。

     

    Abstract: A method was established for the determination of Sudan dyes in foods by special solid phase extraction cartridges combined with high performance liquid chromatography. Samples were extracted with n-hexane,purified and enriched by the solid phase extraction cartridges for Sudan dyes. Afterwards,the elution was dried by the rotary evaporation in a water bath at 40℃ and dissolved with methyl tertiary butyl ether-methanol(4:6 of volume ratio)to a constant volume. Sample solution was separated by Waters Symmetry C18 column(150 mm×4.6 mm,5 μm)with the gradient elution using the mobile phase of acetonitrile-water. Sudan dyes were detected with diode array detection and qualified by the external standard method. Results showed that the linear correlation coefficients of the four Sudan dyes were all above 0.9999 within 0.16~2.56 μg/mL. Detection limits for different kinds of foods were 2.3~9.7 mg/kg. Various brands of SPE cartridges for Sudan dyes had diverse abilities to remove matrix interferences and enrich target analytes,and the suitable SPE cartridge could be selected according to food types. ProElut SDH SPE column was generally suitable for the pretreatment of different kinds of foods. CNW Poly-sery MIP-SDR SPE column was available to the pretreatment of most foods except chili powder. Cleanert Sudan SPE column was applicable for the pretreatment of light-colored and low-fat foods. After treated by ProElut SDH SPE cartridges,recoveries of 6 kinds of foods at the spiked level of 2.0 mg/kg were 83.7%~91.1%,and the relative standard deviations were 2.4%~6.2%(n=6). The method is good at purification and enrichment. Compared with GB/T 19681-2005,it has advantages such as easy operation,good repeatability,high accuracy,short analysis time,solvent saving.

     

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