摘要
建立了超高效液相色谱快速测定马口铁罐包装内涂层中痕量游离甲醛的方法.采用2,4-二硝基苯肼与游离痕量甲醛衍生化,对2,4-二硝基苯肼衍生试剂浓度、衍生化反应条件、衍生化溶液稳定时间及过滤条件等样品前处理条件进行了优化.研究结果表明衍生化条件变化对痕量甲醛衍生化影响明显,对高浓度甲醛则无显著影响.方法检出限为0.001mg/L,定量限为0.004mg/L,回收率为83.6%-102.4%.经实验室内和7家第三方认可实验室验证,实验结果实验室内相对标准偏差RSD 1.54%-2.62%,实验室间1.83%-4.78%.与其他方法相比本方法在痕量甲醛水平检测时仍具有检出限低、操作简便、快速、稳定等特点,并可应用需要测定痕量甲醛的其它领域.
Here a new method is proposed to determine trace free formaldehyde in the inside coating layer of tin can by ultra high performance liquid chromatography （HPLC）. Derivatization conditions, inclu- ding the concentration of 2,4-Dinitrophenylhydrazine, reaction time, and the type of filter were opti- mized. The results show that the derivatization condition is as key factor to the determination of trace formaldehyde, but few effect to high concentration formaldehyde. The limit of dection and limit （LOD） of quant 6% tol 4.78%, fields. ity （LOQ） are 0. 001 and 0. 004 mg/L, respectively. The recovery of m 02.4%. RSD （relative standard deviation） of inter and intra Lab are 2.28 respectively. The method can be applied to the determination of trace ethod ranges from 83. %-4.78G and 1.83%- formaldehyde in other
出处
《四川大学学报（自然科学版）》
CAS
CSCD
北大核心
2014年第6期1262-1266,共5页
Journal of Sichuan University(Natural Science Edition)
基金
国家自然科学基金(201147005)
国家质检总局科研专项(2014IK073)
关键词
超高效液相色谱
甲醛
2
4-二硝基苯肼
痕量
马口铁罐
涂层
Ultra high performance liquid chromatography
Formaldehyde
2,4-Dinitrophenylhydrazine
Trace
Tin can
Coating
