High Performance Liquid Chromatography-Electrospray Ionization-Mass Spectrometric Analysis of Bilobalide and Ginkgolides in Ginkgo biloba L. Leaves

The ginkgo terpenoids including bilobalide and ginkgolides are the main pharmaceutical components in the leaves or extracts of Ginkgo biloba L. In this paper, the analysis of bilobalide and ginkgolides in leaves of Ginkgo biloba L. by high performance liquid chromatography (HPLC)-electrospray ionization (ESI)-mass spectrometry (MS) was carried out. The separation was performed on Inertsil ODS3 column with methanol-water (36:64) as mobile phase, with 1 mL·min -1 of flow rate at 35℃. Then the mass spectrum analysis was conducted by ZMD micromass electrospray ionization (ESI)-mass spectrometer (MS). The HPLC total ion chromatogram and selected ion chromatogram (with 325, 407, 423, 439 of m/z) of the sample and ESI-/MS mass spectra of the peaks in the chromatograms were obtained. So bilobalide, ginkgolide A, B, C and J in Ginkgo biloba L. leaves were identified. The method is easy and rapid, with a good accuracy.

Simple Method for Simultaneous Quantitation and Fingerprint Analysis of Ginkgo biloba Tablets by High Performance Liquid Chromatography-UV-Evaporative Light Scattering Detector

By optimizing the separation and analytical conditions, a reliable, simple and accurate high-performance liquid chromatography（HPLC） method coupled with ultraviolet（UV） and evaporative light scattering detector（ELSD） was developed for the simultaneous determination of lactones and flavonoid, that is, bilobalide, ginkgolide A, ginkgolide B, and rutin, in more than 10 batches of Ginkgo biloba tablets from different pharmaceutical companies. The method could also be applied to fingerprint research, for a more general evaluation of the quality of this preparation. The separation of the components was achieved on a Hanbon C18 column with gradient elution using water and methanol containing 0.1% trifluoroacetic acid（TFA）. The column temperature was 30 ℃ and the flow-rate of the mobile phase was 0.6 mL/min. The drift tube temperature of the ELSD was set at 100 ℃, and the nitrogen flow-rate was 2 L/min. Good linear relationships were shown with correlation coefficients for analytes exceeding 0.9913. The limits of detection（LODs, S/N=3） and the limits of quantitation（LOQs, S/N=10） were 0.00887-0.0508 μg/μL and 0.0171- 0.0636 μg/μL, respectively, on the column. The relative standard deviations（RSD） of the analytes were less than 3.61% for intraday and 3.70% for interday, respectively. The average recovery rates obtained were in the range of （97.3±4.3）% to （101.9±3.1）% for all the compounds. The results of quantitative and fingerprint analysis proved that the contents of the components were totally similar in the preparation of Ginkgo biloba tablets from the same pharmaceutical company; whereas, they varied significantly in the preparations of Ginkgo biloba tablets from different companies.

PURIFICATION OF GINKGO LEAVES EXTRACT WITH MACROPOROUS ADSORBENT BASED ON UREA-FORMALDEHYDE CONDENSED POLYMERS

The relationship between the adsorption properties for the active components of ginkgo leaves and the structure of the adsorbents based on urea-formaldehyde condensed polymers was investigated .The results revealed that these adsorbents showed very hjgh adsorption selectivity for both flavonol glycosides and terpene lactones contained in ginkgo leaves. Thus, an adsorption separation procedure for purification of ginkgo leaves extracts was developed.

Comprehensive analysis of chemical constituents in Xingxiong injection by high performance liquid chromatography coupled with mass spectrometry

Xingxiong injection(XXI) is a widely used Chinese herbal formula prepared by the folium ginkgo extract and ligustrazine for the treatment of cardiovascular and cerebrovascular diseases. Compared with the pharmacological studies, chemical analysis and quality control studies on this formula are relatively limited. In the present study, a high performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry(HPLC-QTOF MS) method was applied to comprehensive analysis of constituents in XXI. According to the fragmentation rules and previous reports, thirty ginkgo flavonoids, four ginkgo terpene lactones, and one alkaloid were identified. A high performance liquid chromatography coupled with triple quadrupole mass spectrometry(HPLC-QQQ MS) method was then applied to quantify ten major constituents in XXI. The method validation results indicated that the developed method had desirable specificity, linearity, precision and accuracy. The total contents of ginkgo flavonoids were about 22.05-25.51 μg·mL-1 and the ginkgo terpene lactones amounts were about 4.41-8.70 μg·m L-1 in six batches of XXI samples, respectively. Furthermore, cosine ratio algorithm and distance measurements were employed to evaluate the similarity of XXI samples, and the results demonstrated a high-quality consistency. This work could provide comprehensive information on the quality control of Xingxiong injection, which be helpful in the establishment of a rational quality control standard.