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15种前列腺素类似物的快速筛查和测定  

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

作　　者：陈安丽[1] 张静[1] 黄子沣 严小红[1] CHEN An-li;ZHANG Jing;HUANG Zi-feng;YAN Xiao-hong(Guangzhou Institute for Drug Control,Guangzhou 510160,China)

机构地区：[1]广州市药品检验所,广东广州510160

出　　处：《分析测试学报》2024年第7期1011-1017,共7页Journal of Instrumental Analysis

基　　金：广州市市场监督管理局科技项目(2022kj28)。

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15种前列腺素类似物的方法。样品以饱和氯化钠作为分散剂(蜡质类样品以四氢呋喃分散),经乙腈提取,离心取上清液过滤后,采用Poroshell 120 EC-C_(18)柱(150 mm×3.0 mm,2.7μm)分离,以5 mmol/L甲酸铵(含0.1%甲酸)-乙腈为流动相梯度洗脱。在ESI正离子模式下,采用Targeted MS/MS模式采集15种前列腺素类似物的质谱信息,构建筛查数据库进行快速筛查,确证后的目标物通过外标法定量。结果表明,15种前列腺素类似物的线性关系良好,相关系数(r^(2))均大于0.99;检出限为0.3~17.6μg/g,定量下限为1.1~58.8μg/g。在低、中、高3个加标水平下,水剂、膏霜、乳类、粉类、凝胶5类化妆品基质的回收率为70.1%~134%,相对标准偏差不大于7.5%。该方法简单高效、准确度好,可用于化妆品中前列腺素类似物的定性确证和定量分析,为化妆品风险识别提供技术支撑。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 15 prostaglandin analogues in cosmetics.The analytes in sample were dis⁃persed in saturated sodium chloride solution(wax samples were dispersed with tetrahydrofuran),then extracted with acetonitrile.After centrifugation and filtration,the UPLC separation of 15 prosta⁃glandin analogues was performed on Poroshell 120 EC-C_(18) column(150 mm×3.0 mm,2.7μm),using 5 mmol/L ammonium formate(containing 0.1%formic acid)solution and acetonitrile as mobile phase by gradient elution.15 prostaglandin analogues were detected by positive ion electrospray ion⁃ization(ESI)in the Targeted MS/MS mode.To construct a screening library with the software by the retention time,exact mass of primary parent ions,isotope abundance ratio and secondary sub-ion li⁃brary matching were collected.The results of matching were used to rapid identification of 15 prosta⁃glandin analogues in cosmetics.The quantification of primary parent ions was performed by external standard method.15 prostaglandin analogues were all well separated.The linear correlation coefficients(r^(2))were more than 0.99.The limits of detection(LODs)ranged of 0.3-17.6μg/g and the lim⁃its of quantitation(LOQs)ranged of 1.1-58.8μg/g.The recoveries at three spiked levels in lotion,cream,emulsion,powder and gel matrices varied from 70.1%to 134%,with relative standard devi⁃ations not more than 7.5%.The established method is rapid,simple and accurate,which is suitable for the screening and determination of 15 prostaglandin analogues in cosmetics,providing technical support for cosmetic risk identification.

关 键 词：超高效液相色谱-四极杆-飞行时间高分辨质谱 快速筛查 化妆品 前列腺素类似物 

分 类 号：O657.7[理学—分析化学] TQ658[理学—化学]