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.
出处
《分析测试学报》
CAS
CSCD
北大核心
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)
作者简介
通讯作者：谭建华，在职博士生，研究方向：有机物检测技术，Tel：020—83300529，E—mail：tanjianhua0734@Miyun．com
