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日用化学工业（中英文）

日用化学工业 ›› 2020, Vol. 50 ›› Issue (1): 59-63.doi: 10.3969/j.issn.1001-1803.2020.01.011

• 分析与检测 • 上一篇    下一篇

高效液相色谱法测定口腔护理产品中卡松含量及质谱确证

王聪1,闫妍1,王超1,王秀娟1,苏宁1(),余梦圆2   

  1. 1. 中国检验检疫科学研究院,北京 100176
    2. 中检科（北京）化妆品技术有限公司,北京 100176
  • 收稿日期:2019-05-14 修回日期:2019-12-25 出版日期:2020-01-22 发布日期:2020-01-16
  • 通讯作者: 苏宁
  • 作者简介:王 聪（1995-），女，河北人，检测工程师，学士，电话：18513944892，E-mail：1170749304@qq.com
  • 基金资助:
    高新技术研究项目资助(1No.RD09)

Determination of kathon content in oral care products by high performance liquid chromatography and verification by HPLC-MS/MS

WANG Cong1,YAN Yan1,WANG Chao1,WANG Xiu-juan1,SU Ning1(),YU Meng-yuan2   

  1. 1. Chinese Academy of Inspection and Quarantine, Beijing 100176, China
    2. Inspection Department （Beijing） Cosmetics Technology Co., Ltd., Beijing 100176, China
  • Received:2019-05-14 Revised:2019-12-25 Online:2020-01-22 Published:2020-01-16
  • Contact: Ning SU

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摘要：

建立了口腔护理产品中卡松含量的高效液相色谱分析方法。以水和甲醇溶解,超声提取过滤后,选用C18 （250 mm×4.6 mm,5 μm）色谱柱,流动相为甲醇和水（45∶55,V/V）,以275 nm波长在15 min内进行定量分析。甲基异噻唑啉酮（MIT）和甲基氯异噻唑啉酮（CMIT）分离效果良好,其中甲基异噻唑啉酮的线性范围为0.07~10 mg/L（R 2>0.999 0）,检出限和定量限分别为0.2和0.7 mg/kg,实际样品中加标回收率和相对标准偏差范围分别为96.1%~101.4%和1.1%~5.6%;甲基氯异噻唑啉酮的线性范围为0.2~30 mg/L（R 2>0.999 0）,检出限和定量限分别为0.6和2 mg/kg,实际样品中加标回收率和相对标准偏差范围分别为96.0%~101.8%和1.0%~2.9%。阳性样品可用液相色谱-串联四级杆质谱（HPLC-MS/MS）进行确证。该分析方法简便、准确、快速,适用于口腔护理产品中卡松含量的测定。

关键词: 卡松, 口腔护理产品, 高效液相色谱, 甲基异噻唑啉酮, 甲基氯异噻唑啉酮, 液相色谱-串联四级杆质谱

Abstract:

A high performance liquid chromatography method for the determination of kathon in oral care products was established. It was dissolved in water and methanol, and after ultrasonic extraction and filtration, a column of C18 column （250 mm×4.6 mm, 5 μm） was used. The mobile phase was methanol and water （45∶55,V/V） and the quantitatively analysis was carried out at a wavelength of 275 nm in 15 minutes. The results show that methylchloroisothiazolone （CMIT） and methylisothiazolone （MIT） have good separation performance, among which the linear range is 0.07-10 mg/L （R 2>0.999 0）. The limits of quantitation （LOQs） and detection （LODs） are 0.7 and 0.2 mg/kg, respectively. The recovery rate of the actual sample is 96.1%-101.4%, and the relative standard deviation （RSDs） is between 1.1% and 5.6%. The linear range of methylchloroisothiazolone is 0.2-30 mg/L （R 2>0.999 0）. The limits of quantitation （LOQs） and detection （LODs） are 2 and 0.6 mg/kg, respectively. The spiked recovery and relative standard deviation range of the actual samples are 96.0%-101.8% and 1.0%-2.9%, respectively. The detection of the kathon sample can be confirmed by liquid chromatography-tandem quadrupole mass spectrometry （HPLC-MS/MS）. The analytical method is simple, accurate and rapid, and it is suitable for the determination of kathon in oral care products.

Key words: kathon, oral care products, liquid chromatography, methylisothiazolinone, methylchloroisothiazolinone, liquid chromatography-tandem quadrupole mass spectrometry

中图分类号: 

  • TQ658.4