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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,p H 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×100 mm,1.7μm)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-QTOF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。
A UPLC method was developed for the determination of baicalin and albic acid in cosmetics and the mass spectrometric method for determination of UPLC-Q-TOF was established. Cosmetics of different matrix types were ultrasonically extracted with methanol-phosphoric acid buffer (9: 1, p H 2.5), demineralized with sodium chloride and eluted with acetonitrile-0.1% formic acid as mobile phase using Waters CSH C18 mm × 100 mm, 1.7μm) column, the target and sample impurities were effectively separated and quantified at 314 nm as the detection wavelength. The correlation coefficient between baicalin and boswelline in the range of 0.05 ~ 10 mg / L was more than 0.999, the recoveries were 92.2% ~ 103.1% and the relative standard deviations were less than 4%. The detection limits were 0.3 mg / kg. At the same time, UPLC-QTOF mass spectrometry confirmation of baicalin and bicine was established. The baicalin and bastardin were confirmed by the accurate masses of precursor ions and ion ions, the molecular weight was less than 5 ppm and the UV absorption The structure of baicalin degradation products was determined by spectroscopy, exact mass number and isotope matching.