Rapid Screening and Determination of 18 Non-steroidal Anti-inflammatory Drugs in Cosmetics by Ultra Performance Liquid Chromatography-Quadrupole-Time-of-flight High-resolution Mass Spectrometry

HUANG Jia-ying; LI Yang-jie; FANG Ji-hui; XIAO Shu-xiong; XU Xin-jun

doi:10.12452/j.fxcsxb.23072703

您当前的位置：

首页 >

文章列表页 >

Rapid Screening and Determination of 18 Non-steroidal Anti-inflammatory Drugs in Cosmetics by Ultra Performance Liquid Chromatography-Quadrupole-Time-of-flight High-resolution Mass Spectrometry

Scientific Papers | 更新时间：2024-02-21

- Rapid Screening and Determination of 18 Non-steroidal Anti-inflammatory Drugs in Cosmetics by Ultra Performance Liquid Chromatography-Quadrupole-Time-of-flight High-resolution Mass Spectrometry
- Journal of Instrumental Analysis Vol. 43, Issue 2, Pages: 269-277(2024)
- 作者机构：
  
  1.中山大学药学院，广东广州 510006
  2.广东省药品检验所，国家药品监督管理局化妆品风险评估重点实验室，广东广州 510163
- 作者简介：
- 基金信息：
- DOI：10.12452/j.fxcsxb.23072703
  CLC： O657.63;TQ658
- Published：15 February 2024，
  
  Received：27 July 2023，
  
  Revised：02 November 2023，
- 稿件说明：
扫描看全文
黄佳颖,李杨杰,方继辉等.超高效液相色谱-四极杆-飞行时间高分辨质谱用于化妆品中18种非甾体抗炎药筛查和测定[J].分析测试学报,2024,43(02):269-277.

HUANG Jia-ying,LI Yang-jie,FANG Ji-hui,et al.Rapid Screening and Determination of 18 Non-steroidal Anti-inflammatory Drugs in Cosmetics by Ultra Performance Liquid Chromatography-Quadrupole-Time-of-flight High-resolution Mass Spectrometry[J].Journal of Instrumental Analysis,2024,43(02):269-277.
黄佳颖,李杨杰,方继辉等.超高效液相色谱-四极杆-飞行时间高分辨质谱用于化妆品中18种非甾体抗炎药筛查和测定[J].分析测试学报,2024,43(02):269-277. DOI： 10.12452/j.fxcsxb.23072703.

HUANG Jia-ying,LI Yang-jie,FANG Ji-hui,et al.Rapid Screening and Determination of 18 Non-steroidal Anti-inflammatory Drugs in Cosmetics by Ultra Performance Liquid Chromatography-Quadrupole-Time-of-flight High-resolution Mass Spectrometry[J].Journal of Instrumental Analysis,2024,43(02):269-277. DOI： 10.12452/j.fxcsxb.23072703.

摘要

建立了超高效液相色谱-四极杆-飞行时间高分辨质谱（UPLC-Q-TOF MS）快速筛查和测定化妆品中18种非甾体抗炎药（NSAIDs）的方法。样品采用60%乙腈水溶液超声提取，以ACQUITY UPLC BEH C

（100 mm×2.1 mm，1.7 µm）色谱柱分离，0.1%甲酸水和0.1%甲酸乙腈为流动相梯度洗脱。在ESI正离子扫描模式下，采用Target MS/MS模式采集化合物的质谱信息构建筛查数据库，以保留时间、一级母离子精确质量数、同位素丰度比和二级子离子谱库匹配进行快速筛查，以基质匹配外标法进行定量分析。结果表明18种化合物的线性关系良好，相关系数（

）均大于0.99；检出限为0.001～0.050 μg/g，定量下限为0.004～0.150 μg/g。低、中、高3个加标水平下，膏霜及水剂两种化妆品基质的平均回收率为70.7%～116%，日内相对标准偏差（RSD，

=6）为0.70%～7.5%，日间RSD（

=3）为3.0%～14%。该方法前处理简单高效、准确度好、分析速度快，筛查结果准确，可用于化妆品中非甾体抗炎药的定性确证和定量分析，为化妆品风险识别提供技术手段。

Abstract

In this study，an ultra performance liquid chromatography-quadrupole-time-of-flight high-resolution mass spectrometry（UPLC-Q-TOF MS） method was developed for the rapid screening and quantitative analysis of 18 non-steroidal anti-inflammatory drugs（NSAIDs） in cosmetics. The chromatographic and mass spectrometric conditions were optimized in detail. The samples were firstly extracted by ultrasonic extraction with 60% acetonitrile aqueous solution，then separated on an ACQUITY UPLC BEH C

column（100 mm×2.1 mm，1.7 µm） by gradient elution，with water and acetonitrile both containing 0.1% formic acid as the mobile phases. The 18 NSAIDs were detected by positive ion electrospray ionization（ESI） in the Target MS/MS mode. The retention time，exact mass number of primary parent ions，isotope abundance ratio and secondary sub-ion library matching were collected to construct a screening library with the software. The results of matching were used to rapid identification of 18 NSAIDs in cosmetics. The quantification of primary parent ions was performed by matrix-matched external standard method. The 18 NSAIDs were all well separated，with good linearity. The linear correlation coefficients（

） were more than 0.99. The limits of detection（LODs） ranged from 0.001-0.050 μg/g and the limits of quantitation（LOQs） ranged from 0.004-0.150 μg/g. The mean spiked recoveries at three spiked levels in cream and lotion matrices ranged from 70.7% to 116%，with intra-day relative standard deviations（RSDs，

=6） of 0.70%-7.5% and inter-day RSDs（

=3） of 3.0%-14%. The 500 batches of cosmetic samples were detected and screened under the same conditions. The TOF MS information，including the retention time，exact mass number of primary parent ions，isotope abundance ratio and secondary sub-ion library，were compared between the cosmetic samples and the standard MS information with PCDL software. Finally，three batches of samples added with acetamidophen were indentified. The amounts of the added drug were very high，indicating high safety risk for cosumers using such cosmetics. With the advantages of simplicity，efficiency and accuracy，the method is suitable for the screening and determination of 18 NSAIDs in cosmetics，providing technical support for cosmetic risk identification.

关键词

化妆品非甾体抗炎药超高效液相色谱-四极杆-飞行时间高分辨质谱

Keywords

cosmeticsnon-steroidal anti-inflammatory drugsultra performance liquid chromatography-quadrupole-time-of-flight high-resolution mass spectrometry

references

Wang H W，Li J Y，Yang Y J，Yu Y G. Prog. Vet. Med.（王海为，李剑勇，杨亚军，于远光. 动物医学进展），2011，32（1）：77-80.

Zhang Y，Peng S F. Pharm. China（张毅，彭双发. 中国药业），2007，（13）：63-64.

Pan S L. J. Guizhou Med. Univ.（潘菽浪. 贵阳医学院学报），2005，（3）：266.

Wu P，Jing W J，Liu J，Song J F. Eval. Anal. Drug-Use Hosp.（吴萍，经纬俊，刘杰，宋金方. 中国医院用药评价与分析），2019，19（8）：1007-1009，1012.

Lu Z P，Cao W. Chin. J. Clin. Ration. Drug Use（卢志品，曹伟. 临床合理用药杂志），2018，11（14）：1-2，7.

Sidhu H S，Sadhotra A. Int. J. Basic Clin. Pharm.，2018，7（10）：1974-1975.

National Medical Products Administration.No.28 Bulletin of the National Medical Products Administration （国家药品监督管理局，国家药品监督管理局2021年第28号通告）.［2021-04-23］.https：//www.nmpa.gov.cn/xxgk/ggtg/hzhpggtg/jmhzhptg/20210428140400103.htmlhttps://www.nmpa.gov.cn/xxgk/ggtg/hzhpggtg/jmhzhptg/20210428140400103.html.

Cen L Y，Xiao S X，Zeng Z J，Chen Z H. Flavour Fragrance Cosmet. （岑立怡，肖树雄，曾子君，陈张好. 香料香精化妆品），2021，（5）：55-59.

Xiao S X，Huang J Y，Zhou Z M，Chen G Q，Qi A M. China Food Drug Adm. Mag. （肖树雄，黄佳颖，周智明，陈桂琴，漆爱明. 中国食品药品监管），2022，（5）：60-65.

Dong Y L，Yuan Y Y，Qiao Y S，Huang C F，Wang H Y. Flavour Fragrance Cosmet. 董亚蕾，袁莹莹，乔亚森，黄传峰，王海燕. 香料香精化妆品），2023，（3）：43-47.

Wang W J，Long L Y，Jiang C J，Li X Y. China Pharm. （王伟姣，龙凌云，姜成君，李晓燕. 中国药师），2020，23（1）：155-160.

Chen C G，Liu M，Li M F，Pang F G，Li L Y. Chin. J. Pharm. Anal.（陈承贵，刘敏，李美芳，庞发根，李兰玉.药物分析杂志），2021，43（3）：515-524.

Sun Z X，Li M，Huang J J，Qian S X，Gu Y N，Li J C. Chin. J. Vet. Drug（孙志轩，李苗，黄婧洁，钱思萱，顾雅妮，李建成. 中国兽药杂志），2023，57（7）：77-86.

Hu X N，Xu H J，Li Y，Guo W L，Ji W H，Wang X. J. Food Saf. Qual.（胡晓楠，徐慧静，李莹，郭文丽，纪卫红，王欣. 食品安全质量检测学报），2022，13（19）：6409-6415.

Wang C，Yu H，Yao W R，Cheng Y L，Guo Y H，Qian H，Tan Z Q，Xie Y F. Spectrosc. Spectral Anal.（王成，于航，姚卫蓉，成玉梁，郭亚辉，钱和，谭志强，谢云飞. 光谱学与光谱分析），2021，41（2）：592-598.

Zhu X H，Li T，Ma P F，Zhu J R，Yan Y，Liu H J. Chin. J. Pharm. Anal.（朱小红，李涛，马鹏飞，朱建荣，颜钰，刘海静. 药物分析杂志），2012，32（10）：1847-1852.

Alatawi H，Hogan A，Albalawi I，O'Sullivan C E，Alsefri S，Wang Y N，Moore E. Electrophoresis，2022，43（20）：1944-1952.

Li J，Zhou Z M，Huang J Y，Xiao S X. Guangdong Chem. Ind.（李静，周智明，黄佳颖，肖树雄. 广东化工），2022，49（5）：164-166.

Xiong S，Liu C Y，Wang Z J，Li H，Ren X D，Wang L，Tian F L，Zhao H B. J. Instrum. Anal. （熊爽，刘成雁，王志嘉，李红，任雪冬，王璐，田福林，赵海波. 分析测试学报），2017，36（8）：980-985.

Dong Y L，Qiao Y S，Huang C F，Wang H Y，Sun L. J. Instrum. Anal.（董亚蕾，乔亚森，黄传峰，王海燕，孙磊. 分析测试学报），2022，41（2）：220-226.

Jia C P，Zhang B，Zhang S S，Zheng J X，Zheng M，Chen W. China Surfactant Deterg. Cosmet（贾昌平，张斌，张珊珊，郑佳新，郑梅，陈卫. 日用化学工业），2022，52（2）：207-213.

Li N，Zhang Y T，Liu L，Shao H，Li H，Li J，Guo Y Z. Chin. Agric. Sci. Bull. （李娜，张玉婷，刘磊，邵辉，李辉，李晶，郭永泽. 中国农学通报），2014，30（27）：299-303.

Dong C C，Hu Y Y，Lü Y N，Song W，Han F，Zheng P，Deng N. Chin. J. Chromatogr.（董婵婵，胡艳云，吕亚宁，宋伟，韩芳，郑平，邓宁. 色谱），2016，34（9）：850-859.

Luo H T，Huang X L，Wu H Q，Zhang Q Y，Zhu Z X，Huang F，Lin X S. Chin. J. Anal. Chem.（罗辉泰，黄晓兰，吴惠勤，张秋炎，朱志鑫，黄芳，林晓珊. 分析化学），2017，45（9）：1381-1388.

National Medical Products Administration.No.268 Bulletin of the National Medical Products Administration（国家药品监督管理局，国家药品监督管理局2015年第268号通告）. ［2015-12-23］.https：//www.nmpa.gov.cn/xxgk/ggtg/hzhpggtg/jmhzhptg/20151223120001986.htmlhttps://www.nmpa.gov.cn/xxgk/ggtg/hzhpggtg/jmhzhptg/20151223120001986.html.

Views

下载量

CSCD

Alert me when the article has been cited

提交

Tools

Publicity Resources

Rapid Screening and Determination of 15 Prostaglandin analogues in Cosmetics by Ultra Performance Liquid Chromatography-Quadrupole-Time-of-flight High-resolution Mass Spectrometry

Determination of 67 Indicative Components from Plant Extracts in Cosmetics by Ultra High Performance Liquid Chromatography- Tandem Mass Spectrometry

Determination of Distearyl Dimethyl Ammonium Chloride in Cosmetics by High Performance Liquid Chromatography-Evaporative Light Scattering Detector

Related Author

CHEN An-li

ZHANG Jing

HUANG Zi-feng

YAN Xiao-hong

ZHANG Qiu-yan

HUANG Fang

LIANG Wei-wei

LIAO Jun-tao

Related Institution

Guangzhou Institute for Drug Control

Guangdong Provincial Engineering Research Center for Quality and Safety of Traditional Chinese Medicine，Guangdong Provincial Key Laboratory of Chemical Measurement and Emergency Test Technology，Institute of Analysis，Guangdong Academy of Sciences（China National Analytical Center，）， Guangzhou

Industrial Products Testing Center，Nanjing Customs

Animal，Plant and Food Inspection Center，Nanjing Customs

Light Industrial Products and Children’s Products Inspection Center，Nanjing Customs

Address：100 Xianlie Middle Road, Guangzhou Postal code：510070
Tel：020-87684776,37656606 Fax：020-87684776 Email：fxcsxb@china.com
Technical support is provided by Beijing Founder electronics co., LTD 粤ICP备12017312号-3 京公网安备11010802024621
It is recommended to read the content of this site in Chrome&IE9+. Please switch to extreme mode in browser 360.
Cookies We use cookies to help provide and enhance our service and tailor content. By continuing, you agree to the use of cookies.

⁰