色谱

色谱 ›› 2012, Vol. 30 ›› Issue (12): 1287-1291.DOI: 10.3724/SP.J.1123.2012.04042

• 研究论文 • 上一篇    下一篇

柱前衍生-萃取阻断反应-高效液相色谱法测定化妆品中游离甲醛

吕春华1*, 黄超群1, 陈梅2, 谢文1, 陈笑梅1   

  1. 1. 浙江出入境检验检疫局, 浙江 杭州 310016; 2. 浙江工业大学化学工程与材料学院, 浙江 杭州 310014
  • 收稿日期:2012-07-22 修回日期:2012-09-10 出版日期:2012-12-28 发布日期:2012-12-19
  • 通讯作者: 吕春华,博士,高级工程师,主要研究方向为理化检验. E-mail: lvch@ziq.gov.cn.
  • 基金资助:

    国家质量监督检验检疫总局课题.

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

Lv Chunhua1*, HUANG Chaoqun1, CHEN Mei2, XIE Wen1, CHEN Xiaomei1   

  1. 1. Zhejiang Entry-Exit Inspection and Quarantine Bureau, Hangzhou 310016, China; 2. College of Chemical Engineering and Materials Science, Zhejiang University of Technology, Hangzhou 310014, China
  • Received:2012-07-22 Revised:2012-09-10 Online:2012-12-28 Published:2012-12-19

PDF

709

被引次数

22

摘要： 建立了柱前衍生化-萃取阻断反应-高效液相色谱(HPLC)测定化妆品中甲醛的方法。化妆品中甲醛检测的难点是: 甲醛缓释剂类防腐剂在衍生过程中释放甲醛,影响游离甲醛的准确测定。以2,4-二硝基苯肼(DNPH)乙腈溶液-磷酸盐缓冲液(pH 2)(1:1, v/v)为提取溶液,于室温下快速衍生2 min后,立即加入二氯甲烷萃取,阻断衍生反应,经乙腈稀释后进行HPLC测定。以Agilent C18柱(250 mm×4.6 mm, 5 μm)为分离柱,乙腈-水(60:40, v/v)为流动相,流速为1.0 mL/min,于355 nm波长下检测。在洗发水、乳液、膏霜、洗手液、牙膏、指甲油、粉饼中分别添加50、100、500、1000 μg/g 4个浓度水平的甲醛,其回收率为81%～106%,相对标准偏差(n=6)＜5.0%。方法的定量限(以信噪比(S/N)＞10计)为50 μg/g。该方法快速、简便、重现性好,且可以有效避免甲醛缓释剂类防腐剂分解释放甲醛,适用于化妆品中游离甲醛的测定。

关键词: 高效液相色谱法, 化妆品, 甲醛缓释剂, 游离甲醛, 柱前衍生

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×4.6 mm, 5 μm) at 30 ℃ 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, 1000 μg/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 μg/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.

Key words: cosmetics, formaldehyde donors, free formaldehyde, pre-column derivatization, high performance liquid chromatography (HPLC)