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丹磺酰肼衍生化-高效液相色谱-荧光检测法测定包装纸中的甲醛和乙醛

[Determination of formaldehyde and acetaldehyde in packaging paper by dansylhydrazine derivatization-high performance liquid chromatography-fluorescence detection].

作者信息

Gong Shuguo, Liang Yong, Tang Liyun, Huang Ping, Dai Yunhui

机构信息

Technology Research & Development Center, Hunan Branch of China Tobacco Industrial Corporation, Changsha 410007, China.

College of Chemistry, Xiangtan University, Key Laboratory of Environment Friendly Chemistry and Application of Ministry of Education, Xiangtan 411105, China.

出版信息

Se Pu. 2017 Jul 8;35(7):755-759. doi: 10.3724/SP.J.1123.2017.03008.

Abstract

A high performance liquid chromatography with fluorescence detection (HPLC-FLD) method was developed for the simultaneous determination of formaldehyde and acetaldehyde in packaging paper by dansylhydrazine (DNSH) derivatization. The samples were extracted by derivatization reagent for 30 min, and derived for 24 h. After purifying treatment with a PSA/C18 cartridge, a Diamonsil C18 column (150 mm×4.6 mm, 5 μ m) was used as stationary phase for separation, the mixtures of acetic acid aqueous solution (pH 2.55)-acetonitrile were used as mobile phases by gradient elution, and the excitation and emission wavelengths were 330 nm and 484 nm, respectively. The results showed that the recoveries of formaldehyde and acetaldehyde spiked in the samples were 81.64%-106.78%, and the relative standard deviations (RSDs) were 2.02%-5.53% (=5). The limits of detection of formaldehyde and acetaldehyde were 19.2 μ g/kg and 20.7 μ g/kg, respectively. The limits of quantification of formaldehyde and acetaldehyde were 63.9 μ g/kg and 69.1 μ g/kg, respectively. The method is simple, sensitive and reproducible. It provides a basic approach for the determination of trace formaldehyde and acetaldehyde.

摘要

建立了一种采用丹磺酰肼(DNSH)衍生化,结合荧光检测的高效液相色谱法(HPLC-FLD),用于同时测定包装纸中的甲醛和乙醛。样品用衍生化试剂萃取30分钟,衍生24小时。经PSA/C18小柱净化处理后,以Diamonsil C18柱(150 mm×4.6 mm,5μm)为固定相进行分离,以乙酸水溶液(pH 2.55)-乙腈混合液为流动相进行梯度洗脱,激发波长和发射波长分别为330 nm和484 nm。结果表明,样品中加标的甲醛和乙醛回收率为81.64%-106.78%,相对标准偏差(RSD)为2.02%-5.53%(n = 5)。甲醛和乙醛的检测限分别为19.2μg/kg和20.7μg/kg。甲醛和乙醛的定量限分别为63.9μg/kg和69.1μg/kg。该方法简便、灵敏、重现性好。为痕量甲醛和乙醛的测定提供了一种基本方法。

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