Department of Pharmacy, School of Stomatology, Fourth Military Medical University, Xi'an, P R China.
J Sep Sci. 2012 Aug;35(16):2054-62. doi: 10.1002/jssc.201200009. Epub 2012 Jul 2.
A sensitive and reliable ultra-high performance liquid chromatography-electrospray ionization-tandem mass spectrometry has been developed and partially validated to evaluate the quality of Semen Cassiae (Cassia obtusifolia L.) through simultaneous determination of 11 anthraquinones and two naphtha-γ-pyrone compounds. The analysis was achieved on a Poroshell 120 EC-C(18) column (100 mm × 2.1 mm, 2.7 μm; Agilent, Palo Alto, CA, USA) with gradient elution using a mobile phase that consisted of acetonitrile-water (30 mM ammonium acetate) at a flow rate of 0.4 mL/min. For quantitative analysis, all calibration curves showed perfect linear regression (r(2) > 0.99) within the testing range. This method was also validated with respect to precision and accuracy, and was successfully applied to quantify the 13 components in nine batches of Semen Cassiae samples from different areas. The performance of developed method was compared with that of conventional high-performance liquid chromatography method. The significant advantages of the former include high-speed chromatographic separation, four times faster than high-performance liquid chromatography with conventional columns, and great enhancement in sensitivity. This developed method provided a new basis for overall assessment on quality of Semen Cassiae.
建立并部分验证了一种灵敏、可靠的超高效液相色谱-电喷雾串联质谱法,用于通过同时测定 11 种蒽醌类化合物和 2 种萘并γ-吡喃酮类化合物来评价决明子(钝叶决明)的质量。分析在 Poroshell 120 EC-C18 柱(100mm×2.1mm,2.7μm;Agilent,美国加利福尼亚州帕洛阿尔托)上进行,采用梯度洗脱,流动相为乙腈-水(30mM 乙酸铵),流速为 0.4mL/min。对于定量分析,所有校准曲线在测试范围内均呈现出完美的线性回归(r2>0.99)。该方法还进行了精密度和准确度验证,并成功应用于从不同地区的 9 批决明子样品中定量测定 13 种成分。与常规高效液相色谱法相比,开发方法的性能得到了比较。该方法的显著优点包括高速色谱分离,与传统柱高效液相色谱相比快四倍,并且灵敏度大大提高。该方法为全面评价决明子的质量提供了新的依据。