摘要
本研究建立高效液相色谱法测定市售白酒中甲醛含量的分析方法。采用乙腈-2,4-二硝基苯肼和乙酸钠混合体系作为衍生液,在60℃水浴中进行衍生,提取样品中的甲醛。生成的衍生物经色谱柱Inertsil ODS-3-C18(4.6 mm×250 mm,5μm)洗脱,流动相为甲醇∶水(68∶32,V∶V),流速1.0 mL/min,柱温40℃,检测波长为360 nm。结果表明,甲醛在0.0125~1.0 mg/L浓度范围内,线性关系良好,3个不同水平的加标回收率为93.27%~98.06%,RSD值为1.98%,检出限为1.5μg/mL,12种市售白酒中的甲醛含量在0.37~12.98 mg/L之间。该方法操作简单,稳定性好,适用于快速检测白酒中甲醛含量。
In this study we established a determination method for formaldehyde content in Baijiu by high performance liquid chromatography. The mixed system of acetonitrile-2,4-dinitrophenylhydrazine and sodium acetate was used as the derivatization solution,and the derivatization was carried out in 60 ℃ water bath to extract the formaldehyde in the sample. The generated derivative was eluted with the chromatographic column Inertsil ODS-3-C18(4.6 mm×250 mm, 5 μm);the mobile phase was methanol-water(68∶32,V∶V);the flow rate was 1.0 mL/min, the column temperature was 40 ℃, and the detection wavelength was 360 nm. The results showed that formaldehyde had good linear relationship in the concentration range of 0.0125 mg/L to 1.0 mg/L, the spiked recovery rate was between 93.27 % and 98.06 %, the RSD value was 1.98 %, and the detection limit was 1.5 μg/mL. The formaldehyde content in the 12 commercially available Baijiu products was between 0.37 mg/L and 12.98 mg/L. The method is simple in operation and has good stability, which is suitable for the rapid detection of formaldehyde content in Baijiu.
作者
胡杨
李先芝
刘洋
林露
石豪
毛琼丽
严玲
HU Yang;LI Xianzhi;LIU Yang;LIN Lu;SHI Hao;MAO Qiongli;YAN Ling(Jing Brand Co.Ltd.,Daye,Hubei 435112;Hubei Key Lab for Quality and Safety Control of Traditional Chinese Medicine and Healthcare Food,Daye,Hubei 435112,China)
出处
《酿酒科技》
2021年第8期114-117,共4页
Liquor-Making Science & Technology
关键词
甲醛
白酒
衍生
高效液相色谱
formaldehyde
Baijiu
derivatization
high performance liquid chromatography
作者简介
胡杨(1993-),男,硕士,研究方向:食品质量控制,E-mail:whhuyang@126.com。;通讯作者:李先芝(1978-),女,土家族,硕士,研究方向:食品质量控制,E-mail:838097968@qq.com。
