CAJ | 학술논문

建立了超高效液相色谱-线性离子阱/静电场轨道阱组合式高分辨质谱联用（ UPLC-LTQ/Orbitrap MS）快速筛查、定性识别化妆品中24种激素的分析方法。不同剂型的化妆品样品经甲醇超声提取，用 Waters ACQUITY UPLC BEH C18色谱柱（50 mm×2.1 mm，1.7μm）分离，以乙腈和0.1％（v/v）甲酸水溶液为流动相进行梯度洗脱。通过静电场轨道阱全扫描得到激素化合物的准分子离子的精确质量数，实现对化妆品中激素的快速筛查；再以保留时间和数据依赖扫描（ data dependent scan）模式获得的子离子质谱图进行定性确证。24种激素化合物的质量准确度误差小于3×10-6（3 ppm）；线性良好，相关系数大于0.99；检出限≤10μg/kg（S/N=3），能满足实际化妆品样品的分析要求。应用该方法对不同剂型的50余种化妆品样品进行筛查分析，结果良好。该方法是化妆品中激素快速筛查、定性识别的有效方法。
건립료초고효액상색보-선성리자정/정전장궤도정조합식고분변질보련용（ UPLC-LTQ/Orbitrap MS）쾌속사사、정성식별화장품중24충격소적분석방법。불동제형적화장품양품경갑순초성제취，용 Waters ACQUITY UPLC BEH C18색보주（50 mm×2.1 mm，1.7μm）분리，이을정화0.1％（v/v）갑산수용액위류동상진행제도세탈。통과정전장궤도정전소묘득도격소화합물적준분자리자적정학질량수，실현대화장품중격소적쾌속사사；재이보류시간화수거의뢰소묘（ data dependent scan）모식획득적자리자질보도진행정성학증。24충격소화합물적질량준학도오차소우3×10-6（3 ppm）；선성량호，상관계수대우0.99；검출한≤10μg/kg（S/N=3），능만족실제화장품양품적분석요구。응용해방법대불동제형적50여충화장품양품진행사사분석，결과량호。해방법시화장품중격소쾌속사사、정성식별적유효방법。
A method of ultra high performance liquid chromatography-linear ion trap/orbitrap high resolution mass spectrometry( UPLC-LTQ/Orbitrap MS)was established to screen and con-firm 24 hormones in cosmetics. Various cosmetic samples were extracted with methanol. The extract was loaded onto a Waters ACQUITY UPLC BEH C18 column(50 mm×2. 1 mm,1. 7 μm) using a gradient elution of acetonitrile/water containing 0. 1%( v/v )formic acid for the separa-tion. The accurate mass of quasi-molecular ion was acquired by full scanning of electrostatic field orbitrap. The rapid screening was carried out by the accurate mass of quasi-molecular ion. The confirmation analysis for targeted compounds was performed with the retention time and qualita-tive fragments obtained by data dependent scan mode. Under the optimal conditions,the 24 hor-mones were routinely detected with mass accuracy error below 3×10-6(3 ppm),and good lineari-ties were obtained in their respective linear ranges with correlation coefficients higher than 0. 99. The LODs( S/N=3)of the 24 compounds were ≤10μg/kg,which can meet the requirements for the actual screening of cosmetic samples. The developed method was applied to screen the hor-mones in 50 cosmetic samples. The results demonstrate that the method is a useful tool for the rapid screening and identification of the hormones in cosmetics.