化妆品中黄芩苷与白鲜碱的超高效液相色谱检测及质谱确证  

Determination of Baicalin and Dictamnine in Cosmetics by UPLC and Their Comfirmations by UPLC-Q-TOF

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

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510110 [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》2014年第12期1399-1403,共5页Journal of Instrumental Analysis

基　　金：国家质检总局科技计划项目(2012QK090);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：建立了化妆品中黄芩苷和白鲜碱的超高效液相色谱（UPLC）检测方法和超高效液相色谱-四极杆串联飞行时间质谱仪（UPLC-Q-TOF）的质谱确证方法.不同基质类型的化妆品经甲醇-磷酸缓冲溶液（9∶1,pH 2.5）超声提取,氯化钠破乳化,以乙腈-0.1％甲酸水溶液为流动相,梯度洗脱,利用Waters CSH C18（2.1 mm ×l00 mm,1.7 μm）色谱柱对目标物和样品杂质进行有效分离,以314 nm为检测波长进行定量测定.黄芩苷和白鲜碱在0.05～10 mg/L范围内均呈良好线性,相关系数大于0.999,方法的回收率为92.2％～103.1％,相对标准偏差小于4％,方法检出限均为0.3 mg/kg.同时建立了对黄芩苷和白鲜碱的UPLC-Q-TOF质谱确证方法,通过一个母离子和子离子的精确质量数对黄芩苷和白鲜碱进行确证,分子质量精确度小于5 ppm,并结合紫外吸收光谱、精确质量数及同位素匹配对黄芩苷的降解产物进行了结构确定.An analytical method was established for the determination of baicalin and dictamnine in cosmetics by ultra performance liquid chromatography （UPLC）.Different types of samples were extracted by ultrasonication with methanol-phosphate buffer solution （9 ∶ 1,pH 2.5）.After demulsified by addition of appropriate NaCl,sample extracts were separated on an ACQUITY UPLCTM CSH C18 column（2.1 mm × 100 mm,1.7 μm,Waters） by gradient elution using acetonitrile-0.1％ fomic acid as mobile phase.The detective wavelength was 314 nm.For the target compouds,the calibration curves were linear in the range of 0.05-10 mg/L,with correlation coefficients more than 0.999.The method limits of detection（LOD,S/N =3） for both were 0.3 mg/kg.The average recoveries ranged from 92.2％ to 103.1％ with relative standard deviations （RSDs） less than 4％.Meanwhile,the confirmed method was developed by ultra-performance liquid chromatography quadrupole-time-of-flight mass spectrometric （UPLC-Q-TOF） with a parent ion and a product ion monitored.The accuracy of molecular ions was less than 5 ppm.By this method,a degradation product of baicalin was also identified.

关 键 词：化妆品 黄芩苷 白鲜碱 超高效液相色谱 超高效液相色谱-四极杆串联飞行时间质谱 

分 类 号：O657.63[理学—分析化学] TQ460.72[理学—化学]