首页|HPLC法测定食品中组胺的研究

HPLC法测定食品中组胺的研究

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食品中组胺含量的检测是食品安全的研究热点.以国标为基础,对测定波长、柱温和流速进行了单因素优化,并用优化条件对基围虾和料酒样品进行检测.样品首先经过0.4mol/L的高氯酸超声提取,正己烷除脂,饱和NaHCO3溶液缓冲后,用10mg/mL丹磺酰氯溶液衍生,在40℃水浴振荡仪中水浴振荡35min,乙腈定容过0.22μm滤膜.在流速为1.0mL/min,检测波长为252nm,柱温为40℃,进样体积为20μL的色谱条件下,通过Agilent C18(4.6mm×250mm,5μm)色谱柱,使用按一定比例混合后的甲基氰溶液和含0.1%乙酸的0.01mol/L的乙酸铵水溶液进行梯度洗脱.结果表明:在该条件下,组胺标准曲线在1.0~50.0μg/mL浓度范围内呈现良好的线性趋势,R2≥0.9999,其样品平均回收率为92.7%~101%,符合GB 27404—2008的相关要求,RSD(n=6)≤3.72%,仪器精密度较好,能够快速、简便、准确测定水产品及液态调味料食品中组胺的含量.
Study of Determination of Histamine in Food by HPLC
The detection of histamine content in food is a research hotspot in the field of food safety. This article opti-mizes the determination wavelength,column temperature,and flow rate based on national standards,and detects samples of shrimp and cooking wine. The sample was first ultrasonically extracted with 0.4 mol/L perchloric acid,degreased with n-hexane,buffered with saturated NaHCO3 solution,and derivatized with 10 mg/mL dansyl chloride solution. The sam-ple was shaken in a 40℃ water bath shaker for 35 min,and acetonitrile was passed through a 0.22 μm filter membrane at constant volume. At a flow rate of 1.0 mL/min,the detection wavelength is 252 nm,column temperature is 40℃. Un-der chromatographic conditions with a sample volume of 20 μL,gradient elution is carried out on Agilent C18(4.6 mm× 250 mm,5 μm) column with mixed methyl cyanide solution and 0.01 mol/L ammonium acetate aqueous solution con-taining 0.1% acetic acid. Results:Under these conditions,the histamine standard curve showed a good linear trend in the concentration range of 1.0~50.0 μg/mL,R2≥0.9999,the measured detection limit level was lower than the theoreti-cal level specified in the national standard,the average recovery rate of samples was 92.7%~101%,which met the rele-vant requirements of GB 27404—2008,RSD(n=6)≤3.72%. The method can quickly,simply and accurately determine the histamine content in aquatic products and liquid seasoning foods.

HPLChistaminedeterminationmethod optimization

陶鑫、王章成、马成章

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武汉生物工程学院食品科技学院,湖北武汉 430415

HPLC 组胺 测定 方法优化

2024

安徽化工
安徽省化工研究院

安徽化工

影响因子:0.229
ISSN:1008-553X
年,卷(期):2024.50(4)