采用快速解析液相色谱/飞行时间质谱法对穿心莲进行定性和定量分析。

Qualitative and quantitative analysis of Andrographis paniculata by rapid resolution liquid chromatography/time-of-flight mass spectrometry.

机构信息

Department of Pharmacy, The First Affiliated Hospital of Harbin Medical University, Harbin 150001, China.

出版信息

Molecules. 2013 Sep 30;18(10):12192-207. doi: 10.3390/molecules181012192.

A rapid resolution liquid chromatography/time-of-flight tandem mass spectrometry (RRLC-TOF/MS) method was developed for qualitative and quantitative analysis of the major chemical constituents in Andrographis paniculata. Fifteen compounds, including flavonoids and diterpenoid lactones, were unambiguously or tentatively identified in 10 min by comparing their retention times and accurate masses with standards or literature data. The characteristic fragmentation patterns of flavonoids and diterpenoid lactones were summarized, and the structures of the unknown compounds were predicted. Andrographolide, dehydroandrographolide and neoandrographolide were further quantified as marker substances. It was found that the calibration curves for all analytes showed good linearity (R² > 0.9995) within the test ranges. The overall limits of detection (LODs) and limits of quantification (LOQs) were 0.02 μg/mL to 0.06 μg/mL and 0.06 μg/mL to 0.2 μg/mL, respectively. The relative standard deviations (RSDs) for intra- and inter-day precisions were below 3.3% and 4.2%, respectively. The mean recovery rates ranged from 96.7% to 104.5% with the relative standard deviations (RSDs) less than 2.72%. It is concluded that RRLC-TOF/MS is powerful and practical in qualitative and quantitative analysis of complex plant samples due to time savings, sensitivity, precision, accuracy and lowering solvent consumption.

建立了一种快速分辨液相色谱/飞行时间串联质谱（RRLC-TOF/MS）方法，用于定性和定量分析穿心莲中的主要化学成分。通过比较保留时间和精确质量与标准品或文献数据，在 10 分钟内可明确或推测地鉴定出 15 种化合物，包括黄酮类和二萜内酯类。总结了黄酮类和二萜内酯类化合物的特征裂解模式，并预测了未知化合物的结构。穿心莲内酯、脱水穿心莲内酯和新穿心莲内酯被进一步作为标志物定量。结果表明，所有分析物的校准曲线在测试范围内均具有良好的线性（R²＞0.9995）。总体检测限（LOD）和定量限（LOQ）分别为 0.02μg/mL 至 0.06μg/mL 和 0.06μg/mL 至 0.2μg/mL。日内和日间精密度的相对标准偏差（RSD）分别低于 3.3%和 4.2%。平均回收率范围为 96.7%至 104.5%，相对标准偏差（RSD）小于 2.72%。结论：由于节省时间、灵敏度、精密度、准确度和降低溶剂消耗，RRLC-TOF/MS 非常适合用于复杂植物样品的定性和定量分析。