College of Science, China Agricultural University, Beijing 100094, China.
Nat Prod Res. 2009;23(18):1689-98. doi: 10.1080/14786410802187742.
Saussurea involucrata produces several bioactive flavonoids that are derived from the phenylpropanoid pathway. To determine these flavonoids, a sensitive high performance liquid chromatography electrospray ionisation mass spectrometry method (LC-ESI-MS) was developed. Chromatographic separation was then performed. The gradient elution was optimised to give high recoveries and satisfactory chromatographic resolution. Flavonoid detection was carried out using an ion trap as mass analyser. Parameters of the mass analyser were optimised. We used the validated LC-ESI-MS method to verify the identities of bioactive compounds, namely apigenin, luteolin, hispidulin, luteolin-7-O-glucoside and rutin. Calibration curves for these five flavonoids were linear in ranges between 5.0 and 500 microg mL(-1). The limit of detection ranged from 1.5 x 10(-4) (for hispidulin) to 6.1 x 10(-3) mg mL(-1) (for rutin). Precision was well within the acceptable range (RSD < 3.0%) and the recovery rate was between 75.3 and 89.8% for each flavonoid. A method validation study showed that the LC/MS technique was a powerful analytical tool for detecting trace amounts of the flavonoid compounds in extracts of S. involucrata.
肉苁蓉产生了几种生物活性黄酮类化合物,这些化合物来源于苯丙素途径。为了确定这些黄酮类化合物,开发了一种灵敏的高效液相色谱-电喷雾离子化质谱法(LC-ESI-MS)。然后进行色谱分离。优化梯度洗脱以获得高回收率和令人满意的色谱分辨率。使用离子阱作为质量分析仪进行黄酮类化合物的检测。对质量分析仪的参数进行了优化。我们使用经过验证的 LC-ESI-MS 方法来验证生物活性化合物的身份,即芹菜素、木樨草素、山柰酚、木樨草素-7-O-葡萄糖苷和芦丁。这五种黄酮类化合物的校准曲线在 5.0 至 500 μg mL(-1) 之间呈线性。检测限范围从 1.5 x 10(-4)(山柰酚)到 6.1 x 10(-3) mg mL(-1)(芦丁)。精密度在可接受范围内(RSD < 3.0%),每种黄酮类化合物的回收率在 75.3%至 89.8%之间。方法验证研究表明,LC/MS 技术是一种强大的分析工具,可用于检测肉苁蓉提取物中痕量的黄酮类化合物。