柱前衍生-高效液相色谱法测定固体胶棒中的游离甲醛  

Determination of free formaldehyde in solid glue sticks by precolumn derivatization-high performance liquid chromatography

作　　者：吴俊威 姚铭栋 王志强[1] WU Jun-wei;YAO Ming-dong;WANG Zhi-qiang(Anyang Municipal Center for Disease Control and Prevention,Anyang,Henan 455000,China)

机构地区：[1]安阳市疾病预防控制中心,河南安阳455000

出　　处：《中国卫生检验杂志》2022年第3期277-279,共3页Chinese Journal of Health Laboratory Technology

基　　金：安阳市2020科技发展计划科技攻关项目(2020-126)。

摘　　要：目的建立固体胶棒中游离甲醛的柱前衍生-高效液相色谱检测方法。方法固体胶棒中的游离甲醛用水进行超声提取,提取液在60℃水浴中与酸性2,4-二硝基苯肼衍生反应20 min,再用二氯甲烷分2次萃取衍生物,合并2次萃取液后过无水硫酸钠柱脱水,氮吹至尽干后用甲醇溶解定容,过0.22μm滤膜后经C_(18)色谱柱分离,高效液相色谱-二极管阵列检测器检测,与标准甲醛衍生物的保留时间对比定性,外标法定量。结果该方法在1.0μg/ml~10μg/ml浓度内呈良好的线性关系,线性相关系数>0.9990,方法检出限为1.0 mg/kg,定量限为3.0 mg/kg,加标回收率为89.6%~104.5%,样品重复测定6次的相对标准偏差(RSD)为2.8%~3.4%。结论该方法的前处理简单,灵敏度高,准确度好,分析速度快,适用于固体胶棒中游离甲醛的分析测试。Objective To establish a method for the determination of free formaldehyde in solid glue sticks by precolumn derivatization-high performance liquid chromatography.Methods The free formaldehyde in solid glue sticks was extracted with water ultrasonically,followed by the extracted formaldehyde was derivatized with acidic 2,4-dinitrophenylhydrazine in a 60℃water bath for 20 minutes,and the derivates were extracted twice with dichloromethane,and then dehydrated with anhydrous sodium sulfate column.After nitrogen blowing to dryness,the residue was dissolved in methanol and filtrated with 0.22μm membrane,and the filtrate was performed on a C;column and analyzed by high performance liquid chromatography with diode array detection.The retention time of the standard formaldehyde derivative was used for qualitative analysis and external standard method was used for quantitative analysis.Results The linear relationship of the method was satisfactory within the range of 1.0μg/ml-10μg/ml,with the correlation coefficient greater than 0.9990.The detection limit of the method was1.0 mg/kg and the limit of quantification was 3.0 mg/kg.The recovery of standard addition was within 89.6%-104.5%,and the RSD was within 2.8%-3.4%.Conclusion The method is simple,sensitive and accurate,and it can be applied to the detection of free formaldehyde in solid glue sticks.

关 键 词：游离甲醛 柱前衍生 固体胶棒 高效液相色谱法 

分 类 号：O657.7[理学—分析化学]