Institute of Chinese Medical Sciences, University of Macau, Macao SAR, P. R. China.
J Sep Sci. 2010 Jun;33(11):1580-6. doi: 10.1002/jssc.201000034.
A fast method for simultaneous determination of five compounds (one coumarin, two alkaloids and two bibenzyls) in Dendrobium spp. using pressurized liquid extraction and ultra-performance liquid chromatography coupled with photo diode array detection was developed. The separation was performed on an Acquity UPLC BEH C(18) column (50 mm x 2.1 mm id, 1.7 microm) with gradient elution of phosphate buffer (pH=7.1, 20 mM) and acetonitrile within 6 min. The method was validated for linearity, LOD and LOQ, precision and accuracy. All calibration curves showed good linearity (R(2) > or = 0.9999) within test ranges. The overall intra- and inter-day variations (RSDs) of five analytes were less than 2.5%, and the detection recoveries were between 95.6 and 102.3%. The developed method was successfully applied to quantitative analysis of five investigated compounds in different species of Dendrobium. The results showed that there were great variations of their contents, though all these materials were officially used as Chinese herb, Shihu. In addition, the chromatographic fingerprints of Dendrobium spp. were also investigated.
建立了一种利用加压液体萃取和超高效液相色谱-光电二极管阵列检测快速测定石斛中 5 种化合物（1 种香豆素、2 种生物碱和 2 种二苄基）的方法。分离在 Acquity UPLC BEH C（18）柱（50mm×2.1mmid，1.7μm）上进行，采用磷酸盐缓冲液（pH=7.1，20mM）和乙腈在 6min 内进行梯度洗脱。该方法对线性、LOD 和 LOQ、精密度和准确度进行了验证。所有校准曲线在测试范围内均表现出良好的线性（R（2）≥0.9999）。5 种分析物的总体日内和日间变异（RSD）均小于 2.5%，检测回收率在 95.6%至 102.3%之间。所建立的方法成功应用于不同种类石斛中 5 种被调查化合物的定量分析。结果表明，尽管所有这些材料都被正式用作中药石斛，但它们的含量存在很大差异。此外，还研究了石斛的色谱指纹图谱。
