德阳市卤肉制品中麦芽酚和乙基麦芽酚的使用调查

Investigation on Maltol and Ethyl Maltol in Stewed Meat Products in Deyang City

建立高效液相色谱-串联质谱法同时测定德阳市卤肉制品中麦芽酚和乙基麦芽酚含量的方法。样品经水分散后,加甲醇超声处理,低温高超离心除杂,经岛津Shim-Pack C18色谱柱分离,以10 mmol/L乙酸铵水溶液(含0.2%甲酸)和甲醇为流动相进行梯度洗脱。采用电喷雾离子源(ESI+)正离子多反应检测模式(MRM)进行监测。结果表明:在优化的条件下,麦芽酚的检出限和定量限分别是24.1μg/kg和80.3μg/kg;乙基麦芽酚的检出限和定量限分别是5.6μg/kg和18.8μg/kg;它们在各自的线性范围为线性关系良好(相关系数r2均大于0.999)。2种香精在3个水平下的加标回收率在92.9%~101.9%之间,相对标准偏差(SRSD)在1.2%~7.4%之间。该方法灵敏、快捷、可靠,可用于卤肉制品中麦芽酚和乙基麦芽酚的快速检测。用该方法分析德阳市48批卤肉制品,结果发现部分样品中乙基麦芽酚含量较高,存在滥用的风险,提示政府应加强监管。

A high-performance liquid chromatography-tandem mass spectrometry method was established to simultaneously determine the content of maltol and ethyl maltol in stewed meat products in Deyang city. After being dispersed in water, the samples were extracted with methanol in ultrasound treatment, followed by low-temperature and ultra-high speed centrifugation for impurity removal. Then, the separation was performed on ShimadzuShim-Pack C_(18)(100 mm×2.1 mm, 2.7 μm) column using a gradient elution program with mobile phase of 10 mmol/L ammonium acetate aqueous solution(containing 0.2% formic acid) and methanol. The components were determined in the mode of electrospray positive ionization(ESI~+) and multiplereaction monitoring(MRM). The results showed that under the optimized experimental condition, the detection limit and quantification limit of maltol were 24.1 μg/kg and 80.3 μg/kg, respectively, while the detection limit and quantification limit of ethyl maltol were 5.6 μg/kg and 18.8 μg/kg, respectively. They showed good linear relationships within their respective linear ranges(correlation coefficients r~2 were all greater than 0.999). The recoveries of the two essences at three levels were 92.9%-101.9%, and the relative standard deviation was 1.2%-7.4%. This method was sensitive, fast, and reliable for rapid detection of maltol and ethyl maltol in stewed meat products. So it was used to analyze 48 batches of stewed meat products in Deyang City, the results showed that some samples had high levels of ethyl maltol, which posed a risk of abuse. Therefore, supervision should be strengthened.