Liquid Chromatography-mass Spectrometry Detection Of Banned Alkaloids In Cosmetics

Nowadays,the development of economy and the satisfaction of material demand promote the development of cosmetics industry.The application of plant extracts as natural nutritional additives has become a hot research hotspot for new product research in cosmetics with huge market potential in recent years,which can not only enhance the efficacy of cosmetics,but also improve the safety of cosmetics.It has been favored by consumers around the wold.Although the natural ingredients in cosmetics are beneficial to human body,natural plants may also introduce other substances,such as toxic alkaloids.This is a kind of plant secondary metabolites and has significant pharmacological activity and toxicity.Long-term use of cosmetics containing toxic alkaloids will bring great harm to the physical and mental health of consumers.For this reason,the"Cosmetics Safety Technical Specifications"?2015 version?issued by the China Food and Drug Administration clearly stipulates that it is a banned component.At present,there are few methods to detect alkaloids in cosmetics,and the types of alkaloids involved are quite few.So,establishing a method to detect alkaloids in cosmetics is very important.The method for the detection of banned alkaloids in cosmetics using liquid chromatography-mass spectrometry was studied.In the first part,a liquid chromatography-tandem mass spectrometry?HPLC-MS/MS?method was developed for the determination of alkaloids in cosmetics,which was high performance and can determine nine banned alkaloids at the same time.Water was selected as dispersant agent,a mixture of Ammonia-methanol?2:98??V/V?solution was selected as extracting agent,meanwhile,n-hexane was adopted for defat treatment,the extraction and purification operations can be accomplished in one step.The 9 alkaloids were analyzed in positive electrospray ionization mode under multiple reaction monitoring?MRM?mode.The rule of mass spectrometry fragmentation of alkaloids was also researched.In this method,the limits of detection?LODs?and the limits of quantitation?LOQs?varied from 0.03 to 0.36?g/kg and varied from 0.1 to 1.2?g/kg respectively.The recoveries were from 85.3%to130.1%,and the RSDs were 1.0%-13.6%.The proposed method in this article was fast,accurate and sensitive,and it was suitable for the detection of the banned alkaloids in cosmetics.In the second part,a method was established by HPLC-MS/MS,which can determine31 alkaloids in essential oil cosmetics simultaneously with high performance.A mixture of methanol-H₂O?3:1,V/V?including 2%formic acid solution was selected as extracting agent,meanwhile,n-hexane was adopted for defat treatment.The chromatographic separation was performed on a C18 column by gradient elution,with water containing 0.2%formic acid-acetonitrile as mobile phases.The 31 alkaloids were analyzed in positive electrospray ionization mode under multiple reaction monitoring?MRM?mode.In this method,the LODs and LOQs ranged from 0.10?g/kg to 3.03?g/kg and 0.32?g/kg to 10.12?g/kg.The recoveries were 63.5%-126%,and RSDs ware 0.73%-17%.The proposed method in this article was suitable for the detection and safety evaluation of alkaloids in cosmetics.In the third part,a HPLC-MS method was established for the determination of 13alkaloids in cosmetics.In this method,super molecular solvent was used as extractant,0.2%formic acid-water acetonitrile was used as mobile phase for gradient elution,a C18 column was used for separation,and mass spectrometry was used for detection.In this experiment,the solvent proportioning and amount of extracting solvet were optimized by orthogonal experiment.The limits of detection?LODs?and the limits of quantitation?LOQs?varied from 0.02 to 1.58?g/kg and varied from 0.06 to 5.26?g/kg respectively.The method has the advantage of less solvent consumption and simple pretreatment,which is in line with the green and scientific conception advocated now.