分光光度法测定海捕虾中4-己基间苯二酚

Determination of 4-hexylresorcinol in marine-capture shrimp by spectrophotometric method

目的 基于分光光度法建立检测海捕虾中4-己基间苯二酚(4-hexylresorcinol,4HR)的分析方法。方法 用乙腈-二氯甲烷溶液提取4HR,经Sep-Pak NH2固相萃取柱净化, 4HR与固蓝RR盐(fast blue RR salt,FBRR)在碱性介质中反应生成红色偶合产物,进行比色定量。结果 本方法在0~90μg/mL范围内具有良好的线性,相关系数r^(2)=0.9998,其检出限和定量限分别是1.019μg/mL和3.087μg/mL。3个不同加标水平(0.5、1.0、2.0μg/g)的平均回收率为86.30%~93.25%,相对标准偏差为1.57%~5.54%。本方法与现行标准GB5009.280—2020《食品安全国家标准食品中4-己基间苯二酚残留量的测定》进行比对,两种方法检测结果无显著性差异(P>0.05)。结论 本法灵敏、准确可靠,可用于海捕虾中4HR的分析检测。

Objective To establish a method for the determination of the content of 4-hexylresorcinol(4HR)in marine-capture shrimp by spectrophotometric method.Methods The 4HR was extracted with acetonitriledichloromethane from sample.After purification by Sep-Pak NH2 solid-phase extraction column,the 4HR coupled with fast blue RR salt(FBRR)in alkaline medium,yielding red coupling product that could be quantified colorimetrically.Results Good linearity was observed for 4HR in the range 0-90μg/mL with a correlation coefficient of 0.9998.The limits of detection and limits of quantitation were 1.019μg/mL and 3.087μg/mL,respectively.The average recoveries were 86.30%‒93.25%and the relative standard deviations were 1.57%‒5.54%at 3 spiked levels of 0.5,1.0,2.0μg/g.Meanwhile,compared with the current standard of GB 5009.280—2020 National food safety standards-Determination of 4HR residues in foods,the results from 2 kinds of methods had no distinguishability(P>0.05).Conclusion The new method is sensitivity,accuracy,credibility,which can be applied for analysis and detection of 4HR residues in marine-capture shrimp.