论文部分内容阅读
目的建立高效液相色谱法检测食品中的甲醛次硫酸氢钠含量。方法样品经磷酸溶液提取,残留在其中的甲醛次硫酸氢钠分解释放出甲醛,甲醛与衍生试剂2,4-二硝基苯肼发生反应,生成黄色的衍生物苯腙,经Eclipse XDB-C_(18)(250 mm×4.6 mm,5μm)色谱柱分离,流动相为乙腈-水(60:40,V:V),柱温为35℃,流速为1.0 m L/min;检测波长为355 nm,经高效液相色谱仪检测。结果本方法优化的实验条件是:磷酸溶液浓度2.0%,衍生剂2,4-二硝基苯肼溶液的浓度为2.0%,60℃水浴中反应30 min;甲醛标准溶液在0~3μg/m L浓度范围内具有良好的线性关系(r=1.00);在5、10和30μg 3个加标水平上的回收率为95.36%~98.20%,相对标准偏差为0.403%~1.05%;检出限为0.17 mg/kg。结论本方法快速准确,适合于测定食品中甲醛次硫酸氢钠的残留量。
Objective To establish a method for the determination of formaldehyde sodium sulfoxylate in food by high performance liquid chromatography. Methods The sample was extracted with phosphoric acid solution, and formaldehyde formaldehyde sodium bisulfite remained in it to decompose to release formaldehyde. The reaction between formaldehyde and 2,4-dinitrophenylhydrazine derivative reagent yielded yellow phenylhydrazone. (250 mm × 4.6 mm, 5 μm). The mobile phase consisted of acetonitrile-water (60:40, V: V) with a column temperature of 35 ℃ and a flow rate of 1.0 mL / nm, detected by high performance liquid chromatography. Results The optimized experimental conditions were as follows: the concentration of phosphoric acid solution 2.0%, the concentration of 2,4-dinitrophenylhydrazine derivatization solution 2.0%, the reaction at 60 ℃ for 30 min; the standard solution of formaldehyde at 0-3 μg / m (R = 1.00). The recoveries were 95.36% ~ 98.20% at three spiked levels of 5, 10 and 30 μg with relative standard deviations of 0.403% ~ 1.05%. The detection limits 0.17 mg / kg. Conclusion The method is rapid and accurate and is suitable for the determination of the residual amount of formaldehyde sodium sulfoxylate in food.