柱前衍生法检测香菇酱中甲醛

Determination of Formaldehyde in Lentinus edodes Sauce by Pre-column Derivatization Method

建立了一种快速测定香菇酱中甲醛的高效液相色谱法。样品经过乙腈-衍生液萃取,萃取时间1 h,萃取温度60℃。取离心后的上清液及用乙腈重复萃取下层溶液,合并定容,过0.22μm滤膜,用高效液相色谱仪分析。色谱条件:色谱柱为Agilent TC-C18(250 mm×4.6 mm,5μm),柱温25℃,流动相为乙腈∶水(体积比为7∶3),流速1.0 mL/min,使用紫外分光光度检测器,检测波长352 nm。结果表明,甲醛含量在0.08~5.00μg/mL范围内具有良好的线性关系,检测限为0.03μg/mL,加标回收率在93.8%~108.1%,日内精密度为5.7%。该方法前处理方便简单,易操作,检测结果准确性高,稳定性好,是一种适用于香菇酱中微量甲醛检测的方法。

A HPLC method for the determination of formaldehyde in Lentinus edodes sauce is developed.The samples are extracted with acetonitrile-derived solution for 1 h at 60℃.The supernatant after centrifugation and the lower solution extracted with acetonitrile are combined with constant volume,being filtered through 0.22μm membrane,and analyzed by high performance liquid chromatography.The chromatographic conditions are as follows:Agilent TC-C18(250 mm×4.6 mm,5μm),the column temperature is 25℃,the mobile phase is acetonitrile and water(with volume ratio of 7∶3),the flow rate is 1.0 mL/min,using ultraviolet spectrophotometric detector,the detection wavelength is 352 nm.The results show that the linear range of formaldehyde content is 0.08~5.00μg/mL,the detection limit is 0.03μg/mL,the recovery rate is 93.8%~108.1%,and the intra-day precision is 5.7%.The method is simple and convenient for pretreatment,easy to operate,the detection results have high accuracy and good stability,it is suitable for the detection of trace formaldehyde in Lentinus edodes sauce.