Tang Dao-Quan, Zheng Xiao-Xiao, Chen Xu, Yang Dong-Zhi, Du Qian
Department of Pharmaceutical Analysis, Xuzhou Medical College, Xuzhou 221004, China.
Key Laboratory of New Drug & Clinical Application, Xuzhou Medical College, Xuzhou 221004, China.
J Pharm Anal. 2014 Apr;4(2):96-106. doi: 10.1016/j.jpha.2013.12.004. Epub 2013 Dec 28.
A quality control (QC) strategy for quantitative and qualitative analysis of "common peaks" in chemical fingerprint was proposed to analyze Yuanhu Zhitong tablet (YZT), using high performance liquid chromatography with diode array detector and tandem mass spectrometry (HPLC-DAD-MS/MS). The chromatographic separation was achieved on an Agilent Eclipse plus C column with a gradient elution using a mixture of 0.4‰ ammonium acetate aqueous (pH 6.0 adjusted with glacial acetic acid) and acetonitrile. In chemical fingerprint, 40 peaks were assigned as the "common peaks". For quantification of "common peaks", the detection wavelength was set at 254 nm, 270 nm, 280 nm and 345 nm, respectively. The method was validated and good results were obtained to simultaneously determine 10 analytes (protopine, jatrorrhizine, coptisine, palmatine, berberine, xanthotoxin, bergapten, tetrahydropalmatine, imperatorin and isoimperatorin). For qualification of "common peaks", 33 compounds including 10 quantitative analytes were identified or tentatively characterized using LC-MS/MS. These results demonstrated that the present approach may be a powerful and useful tool to tackle the complex quality issue of YZT.
采用配有二极管阵列检测器和串联质谱的高效液相色谱法（HPLC-DAD-MS/MS），提出了一种化学指纹图谱中“共有峰”定量和定性分析的质量控制（QC）策略，用于分析元胡止痛片（YZT）。色谱分离在安捷伦Eclipse plus C柱上进行，使用0.4‰醋酸铵水溶液（用冰醋酸调节pH至6.0）和乙腈的混合物进行梯度洗脱。在化学指纹图谱中，40个峰被指定为“共有峰”。对于“共有峰”的定量分析，检测波长分别设置为254 nm、270 nm、280 nm和345 nm。该方法经过验证，同时测定10种分析物（原阿片碱、药根碱、黄连碱、巴马汀、小檗碱、花椒毒素、佛手柑内酯、延胡索乙素、欧前胡素和异欧前胡素）获得了良好结果。对于“共有峰”的定性分析，使用LC-MS/MS鉴定或初步表征了包括10种定量分析物在内的33种化合物。这些结果表明，本方法可能是解决YZT复杂质量问题的有力且有用的工具。
