Shi Qirong, Yan Shikai, Liang Mingjin, Yang Yun, Wang Yan, Zhang Weidong
School of Pharmacy, Second Military Medical University, Shanghai 200433, PR China.
J Pharm Biomed Anal. 2007 Feb 19;43(3):994-9. doi: 10.1016/j.jpba.2006.09.028. Epub 2006 Nov 3.
High-performance liquid chromatography (HPLC) coupled with electrospray tandem mass spectrometry (ESI-MS-MS) and diode array detection (DAD) was used to identify and simultaneously determine eight major ingredients in Radix Tinosporae. The assay was performed on a Diamonsil C(18) analytical column with a gradient solvent system of A (water containing 0.2% formic acid, 20mM ammonium acetate) and B (methanol/acetonitrile=1/1, v/v). The 217, 248, 270 and 347 nm, respectively, were chosen as the monitoring wavelengths to determine four structural types of components, say columbin, phytoecdysteroids (including 20-hydroxyecdysone, 2-deoxy-20-hydroxyecdysone 3-O-beta-d-glucopyranoside and 2-deoxy-20-hydroxyecdysone), menisperine and protoberberine alkaloids (including columbamine, jatrorrhizine and palmatine). This method was validated in respect to precision, repeatability and accuracy, and was successfully applied to quantify the eight components in 39 batches of R. Tinosporae for quality control purpose. The results indicated that the proposed method could be readily utilized as a quality control method for traditional Chinese medicine (TCM).
采用高效液相色谱(HPLC)与电喷雾串联质谱(ESI-MS-MS)及二极管阵列检测(DAD)联用的方法,对金果榄中的8种主要成分进行鉴定并同时测定。分析在Diamonsil C(18)分析柱上进行,流动相A为含0.2%甲酸、20mM乙酸铵的水,流动相B为甲醇/乙腈=1/1(v/v)的混合溶液,采用梯度洗脱。分别选择217、248、270和347nm作为监测波长,测定4种结构类型的成分,即古伦宾、植物蜕皮甾类(包括20-羟基蜕皮甾酮、2-脱氧-20-羟基蜕皮甾酮3-O-β-D-葡萄糖苷和2-脱氧-20-羟基蜕皮甾酮)、蝙蝠葛碱和原小檗碱类生物碱(包括黄连碱、药根碱和巴马汀)。该方法在精密度、重复性和准确性方面得到验证,并成功应用于39批金果榄中8种成分的含量测定以进行质量控制。结果表明,所建立的方法可作为一种中药质量控制方法。