1.中国食品药品检定研究院/国家药品监督管理局化妆品研究与评价重点实验室,北京 100050
2.湖南省药品检验检测研究院,湖南 长沙 410001
路 勇,博士,教授级高级工程师,研究方向:分析化学及食品、化妆品监管,E - mail:luyong0560@126.com
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王欣然,尹伟成,王海燕等.超高效液相色谱-四极杆飞行时间质谱法快速筛查睫毛用化妆品中前列腺素F2α类化合物[J].分析测试学报,2023,42(01):55-61.
WANG Xin-ran,YIN Wei-cheng,WANG Hai-yan,et al.Rapid Screening of Prostaglandin F2α Compounds in Eyelash Cosmetics by Ultra-performance Liquid Chromatography- Quadrupole Time-of-flight Mass Spectrometry[J].Journal of Instrumental Analysis,2023,42(01):55-61.
王欣然,尹伟成,王海燕等.超高效液相色谱-四极杆飞行时间质谱法快速筛查睫毛用化妆品中前列腺素F2α类化合物[J].分析测试学报,2023,42(01):55-61. DOI: 10.19969/j.fxcsxb.22080101.
WANG Xin-ran,YIN Wei-cheng,WANG Hai-yan,et al.Rapid Screening of Prostaglandin F2α Compounds in Eyelash Cosmetics by Ultra-performance Liquid Chromatography- Quadrupole Time-of-flight Mass Spectrometry[J].Journal of Instrumental Analysis,2023,42(01):55-61. DOI: 10.19969/j.fxcsxb.22080101.
采用超高效液相色谱-四极杆飞行时间质谱(UPLC-Q-TOF MS/MS)技术,建立了睫毛用化妆品中9种前列腺素F2α类化合物(比马前列素、曲伏前列素、他氟前列素、他氟乙酰胺、拉坦前列素、比马前列素酸甲基酯、氯前列醇异丙基酯、15-酮-曲伏前列素、比马酰胺)的快速定性筛查方法。样品经乙腈超声提取,采用Waters ACQUITY UPLC BEH C,18,(2.1 mm × 100 mm,1.7 μm)色谱柱,以2 mmol/L甲酸铵水溶液(含0.05%甲酸)-乙腈为流动相,分离后进入四极杆飞行时间质谱,采用电喷雾离子源正离子模式(ESI+),以MS,E,模式进行数据采集,建立了9种前列腺素F2α类化合物的筛查数据库。9种化合物在各自质量浓度范围内线性关系良好,相关系数(,r,2,)均大于0.99,检出限为0.075 ~ 0.75 μg/g,定量下限为0.25 ~ 2.5 μg/g。所建立的筛查数据库无需对照品即可对化妆品中的9种前列腺素F2α类化合物进行筛查。结果表明,该方法特异性良好,应用于48批睫毛类化妆品的定性筛查具有良好的选择性,可为化妆品中前列腺素F2α类化合物的筛查分析提供技术支持。
A high-throughput method for rapid and qualitative screening of nine prostaglandin F2α compounds,i.e. bimatoprost,travoprost,tafluprost,tafluprost ethyl amide,latanoprost,bimatoprost acid methyl ester,cloprostenol isopropyl ester,15-keto travoprost,N-norbimatoprost in eyelash cosmetics was established by ultra-performance liquid chromatography-quadrupole time-of-flight mass spectrometry(UPLC-Q-TOF MS/MS).The samples were ultrasonically extracted with acetonitrile,separated on a Waters ACQUITY UPLC BEH C,18,(2.1 mm × 100 mm,1.7 μm) chromatographic column with 2 mmol/L ammonium formate aqueous solution containing 0.05% formic acid-acetonitrile as the mobile phase,then data-acquisitioned by quadrupole time-of-flight mass spectrometry in MS,E, mode using electrospray ionization source in positive ion mode(ESI+),and a high-throughput screening database for 9 prostaglandin F2α compounds was established.There were good linear relationships for the 9 analytes in their respective concentration ranges,with correlation coefficients(,r,2,) all greater than 0.99.The detection limits and the quantitation limts of 9 analytes were in the ranges of 0.075-0.75 μg/g and 0.25-2.5 μg/g,respectively.The screening database collected and established by high-resolution mass spectrometry can screen 9 kinds of prostaglandin F2α compounds in cosmetics without reference substances.The results showed that the established method has good selectivity in high-throughput qualitative screening of 48 batches of eyelash cosmetics with good specificity.The method is suitable for the screening and analysis of prostaglandin F2α compounds in cosmetics,and it could provide a technical support for the qualitative analysis of five prostaglandin F2α compounds in cosmetics.
前列腺素F2α化妆品超高效液相色谱-四极杆飞行时间质谱
prostaglandin F2αcosmeticsultra-performance liquid chromatography-quadrupole time-of-flight mass spectrometry
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