Determination of 6 Analgesic Drugs in Cosmetics by Ultra-high Performance Liquid Chromatography£­Tandem Mass Spectrometry

KeyWord:ultra-high performance liquid chromatography£­tandem mass spectrometry£¨UHPLC£­MS/MS£©  cosmetics  analgesic  drugs

Abstract:

      A method was developed for the simultaneous determination of six illegally added analgesic drugs£¬i.e aminopyrine£¬phenacetin£¬diclofenac sodium£¬indometacin£¬phenylbutazone and chlorpheniramine in cosmetics by ultra-high performance liquid chromatography£­tandem mass spectrometry£¨UHPLC£­MS/MS£©£®Four kinds of cosmetics such as cream£¬facial mask£¬gel and spray were selected as the representative matrixes£®The sample pretreatment conditions were optimized in detail£®The cosmetic samples were firstly extracted with acetonitrile by ultrasonic-assisted liquid£­liquid extraction£¬then separated on an ACQUITY UPLC BEH C18 column£¨2.1 mm ¡Á 100 mm£¬1.7 ¦Ìm£© by gradient elution£¬with acetonitrile and water both containing 5 mmol/L ammonium acetate as the mobile phases at a flow rate of 0.3 mL/min and an injection volume of 10 ¦ÌL£¬and finally detected by tandem mass spectrometry under multiple reaction monitoring£¨MRM£© scanning mode£®Retention times and charge£­mass ratio of the compounds£¨parent ion and two daughter ions£© were used for qualitative analysis£®Quantitative analyses were carried out by the matrix standard curves using the peak areas of the daughter ions with higher intensity£®The results showed that there were good linear relationships for six compounds in the range of 5£­200 ¦Ìg/L with their correlation coefficients£¨r£© larger than 0.99£®The limits of detection£¨LOD£© and limits of quantitation£¨LOQ£© of the method were 0.15 ¦Ìg/g and 0.50 ¦Ìg/g£¬respectively£®The recoveries at three spiked levels for the six components in four matrixes ranged from 75.0% to 120%£¬with intra-day relative standard deviations£¨RSD£© not more than 7.9% and inter-day RSD no more than 9.7%£®With the advantages of simplicity£¬high sensitivity and accuracy£¬this method is suitable for the determination of analgesic chemical components in various cosmetics substrates£¬and it also provides a technical support for the safety supervision of cosmetics.