超高效液相色谱-四极杆串联飞行时间质谱法鉴定育发化妆品中4种植物功效成分  

Identification of Four Active Constituents in Hair Growth Cosmetics by Ultra Performance Liquid Chromatography Coupled with Quadrupole Time-of-Flight Mass Spectrometry

作　　者：谢文缄 熊小婷[1] 席绍峰[1,2] 李慧勇[1] 谭建华[1,2] 王继才[1] 赵田甜[1] 郭长虹[1] 

机构地区：[1]广州质量监督检测研究院国家化妆品质量监督检验中心(广州),广东广州510611 [2]华南农业大学资源环境学院,广东广州510642

出　　处：《分析测试学报》2016年第2期164-171,共8页Journal of Instrumental Analysis

基　　金：广州市质量技术监督局科技项目(2014KJ39);国家质量监督检验检疫总局公益性行业科研专项(2012104013-3)

摘　　要：建立了固相萃取/超高效液相色谱-四极杆飞行时间质谱（UPLC-QTOF-MS）鉴定育发化妆品中4种植物功效成分（槲皮苷、何首乌苷、芦丁和柚皮苷）的分析方法。样品采用甲醇超声提取,上清液经2%/甲酸水溶液稀释后上PAX阴离子固相萃取柱净化。以甲醇和0.002%甲酸水溶液为流动相,梯度洗脱,在CSH C18色谱柱（2.1 mm×50 mm,1.7μm,Waters）上分离,于UPLC-QTOF-MS负离子模式下进行检测。槲皮苷、何首乌苷和芦丁采用外标法定量测定;5%氨水溶液条件下,柚皮苷因在PAX上的吸附过程中结构转化为柚皮苷查尔酮,只能进行定性鉴定。在优化条件下,槲皮苷、何首乌苷和芦丁在5~200μg·L-1浓度范围内均呈良好线性,相关系数大于0.999;方法定量下限（LOQ,S/N=10）为0.03~0.1 mg·kg-1;在洗发水基质中的加标回收率为80.9%~104.7%,相对标准偏差（n=6）不大19.6%。该方法准确、适用性强,已成功应用于育发化妆品中槲皮苷、何首乌苷和芦丁的定性定量检测以及柚皮苷的定性鉴定。A method for the determination of four active constituents（ i. e. 2,3,5,4＇-tetrahydroxy stilbene-2-Ο-β-D-glucoside（ THS- GLU）,quercetin-3-rhamnoside（ QR）,rutin（ RT） and naringin（ NG）） in hair growth cosmetics was developed by strong anion exchange- solid phase extraction（ SPE） combined with ultra performance liquid chromatography quadrupole- time- of- flight mass spectrometry（ UPLC- QTOF- MS）. The sample was ultrasonically extracted with methanol,and purified with SPE（ PAX,500 mg /6 m L） cartridge. Chromatographic separation was conducted on a UPLC CSH C18（ 2. 1 mm × 50 mm,1. 7 μm,Waters） column by gradient elution using methanol and0. 002% formic acid solution as mobile phases. The MS analysis was carried out in electrospray ionization operated in negative mode. THS- GLU,QR and RT were quantified by the external standard method. NG, which arised configuration conversion to naringin chalcone, was just identified by qualitative analysis. Under the optimal conditions,satisfactory linearities（ r2 0. 999） for three compounds were obtained for all analytes in the concentration range of 5- 200 μg / L. Limits of quantitation（ S /N = 10） were in the range of 0. 03- 0. 1 mg·kg- 1. Recoveries at three spiked levels were in the range of 80. 9%- 104. 7% with relative standard deviations（ RSD,n = 6） not more than 19. 6%.This method was accurate and applicable,and was succcessfully applied in the determination of THS- GLU,QR,RT and the identification of NG in hair growth cosmetics.

关 键 词：固相萃取(SPE) 超高效液相色谱-四极杆飞行时间质谱(UPLC-QTOF-MS) 育发化妆品 功效成分 

分 类 号：O657.63[理学—分析化学] TQ658[理学—化学]