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柱前衍生化、萃取抑制-高效液相色谱法测定化妆品中的游离甲醛

[Determination of free formaldehyde in cosmetics by pre-column derivatization, extraction inhibition and high performance liquid chromatography].

作者信息

Lü Chunhua, Huang Chaoqun, Chen Mei, Xie Wen, Chen Xiaomei

机构信息

Zhejiang Entry-Exit Inspection and Quarantine Bureau, Hangzhou 310016, China.

出版信息

Se Pu. 2012 Dec;30(12):1287-91. doi: 10.3724/sp.j.1123.2012.04042.

Abstract

Pre-column derivatization and inhibition by solvent extraction were applied to determine free formaldehyde in cosmetics by high performance liquid chromatography (HPLC). Due to the rapid decomposition of formaldehyde donors in the derivatization, it is hard to detect the amount of the free formaldehyde in cosmetics. The formaldehyde directly reacted with 2,4-dinitrophenylhydrazine in acetonitrile-phosphate buffer (pH 2) (1:1, v/v) solution for 2 min, then dichloromethane extraction was used to induce the decomposition of formaldehyde donors. The extract was diluted with acetonitrile and then determined by HPLC. The formaldehyde derivative was separated on an Agilent C18 column (250 mm x 4.6 mm, 5 microm) at 30 degrees C with acetonitrile-water (60:40, v/v) as mobile phase at a flow rate of 1.0 mL/min, and detected at the wavelength of 355 nm. The recoveries were from 81% to 106% at the spiked levels of 50, 100, 500, 1 000 microg/g of formaldehyde in shampoo, milk, cream, hand cleaner, toothpaste, nail polish, powder separately, and the relative standard deviations (n = 6) were less than 5.0%. The limit of quantification of the formaldehyde in cosmetics was 50 microg/g. The method has been applied to the determination of free formaldehyde in real samples and the results showed that the release by formaldehyde donors was inhibited. The method has the advantages of simple operation, good accuracy and meets the requirement of determination of free formaldehyde in cosmetics.

摘要

采用柱前衍生化结合溶剂萃取抑制法,通过高效液相色谱(HPLC)测定化妆品中的游离甲醛。由于甲醛供体在衍生化过程中快速分解,难以检测化妆品中游离甲醛的含量。甲醛在乙腈 - 磷酸盐缓冲液(pH 2)(1:1,v/v)溶液中与2,4 - 二硝基苯肼直接反应2分钟,然后用二氯甲烷萃取以促使甲醛供体分解。萃取液用乙腈稀释后,通过HPLC测定。甲醛衍生物在安捷伦C18柱(250 mm×4.6 mm,5 µm)上于30℃分离,以乙腈 - 水(60:40,v/v)为流动相,流速为1.0 mL/min,在355 nm波长处检测。在洗发水、乳液、面霜、洗手液、牙膏、指甲油、散粉中分别添加50、100、500、1000 μg/g甲醛的加标水平下,回收率为81%至106%,相对标准偏差(n = 6)小于5.0%。化妆品中甲醛的定量限为50 μg/g。该方法已应用于实际样品中游离甲醛的测定,结果表明甲醛供体的释放受到抑制。该方法操作简便、准确度高,满足化妆品中游离甲醛测定的要求。

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