Influence of ultrafiltration membrane on ophiopogonins and homoisoflavonoids in Ophiopogon japonicus as measured by ultra-fast liquid chromatography coupled with ion trap time-of-flight mass spectrometry / 中国天然药物

Ultrafiltration is one of the most fascinating technologies, which makes it possible to improve the quality of traditional medicines for application in the pharmaceutical industry. However, researchers have paid little attention to the effect of ultrafiltration membrane on traditional medicines chemical constituents. In this work, Ophiopogon japonicus (L.f) Ker-Gawl. was used as an example to illuminate the influence of ultrafiltration with different material and molecular weight cut-off (MWCO) membrane on natural chemical constituents as measured by ultra-fast liquid chromatography coupled with ion trap time-of-flight mass spectrometry (UFLC-IT-TOF/MS). Our results indicated that ultrafiltration membrane significantly impacted homoisoflavonoids, especially homoisoflavonoids that were almost completely retained on the polyethersulfone (PES) membrane. We also found that the larger number of aglycone hydroxy and sugar moiety in steroid saponins, the higher the transmittance. Furthermore, the passage rate (%) of ophiogenin type saponins was higher than that of others. The possible adsorptive mechanisms were hydrogen bonding, hydrophobic interactions, and benzene ring interaction by π-π stacking. In conclusion, it is crucial to choose appropriate ultrafiltration membrane based on the characteristics of produce products for application of ultrafiltration technique.

Characterization of metabolites in rats after gavage of two lignans from fruits of Vitex negundo var. cannabifolia by UFLC-IT-TOF-MS / 中草药

Objective: To investigate in vivo metabolic profiles of two lignans, 6-hydroxy-4-(4-hydroxy-3-methoxyphenyl)-3- hydroxymethyl-7-methoxy-3,4-dihydro-2-naphthaldehyde (VB-1) and vitedoin A (VB-2) in the rats. Methods: A UFLC-IT- TOF-MS method was applied to characterize the prototypes and metabolites of VB-1 and VB-2 in rat feces, urine, bile, and plasma after oral administration. Results: Eleven metabolites of the two parent compounds were detected and two prototypes were identified unambiguously by comparing with references. Analysis of metabolites revealed that glucuronidation, sulfation, and hydroxylation were major biotransformation pathways of two lignans. Conclusion: In this study, under the analysis of metabolites of two lignans, its in vivo metabolic process is basically clarified. The results could be helpful for the further pharmacokinetics and pharmacological evaluations of VB-1 and VB-2.

UFLC fingerprint of Huoxiang Zhengqi Dripping Pill / 中草药

Objective: To establish the ultra-fast liquid chromatographic (UFLC) fingerprint of Huoxiang Zhengqi Dripping Pill (HZDP) for evaluating the quality of the preparation. Methods: The UFLC separation was achieved on an Waters Acquity UPLC BEH C18 column (100 mm × 2.1 mm, 1.7 μm) with acetonitrile (A)-0.2% formic acid solution (B) as mobile phase at the flow rate of 0.4 mL/min by gradient elution of 0-6 min, 10% →15% A, 6-9 min, 15% →20% A, 9-14 min, 20% →30% A, 14-19 min, 30% → 50% A, 19-21 min, 50% →65% A, 21-26 min, 65% →75% A, 26-28 min, 75% A, 28-30 min, 75% →10% A, 30-32 min, 10% A. The column temperature was 30 ℃. The UV detection wavelength was 300 nm. The similarity of 11 batches of HZDP was analyzed with similarity evaluation system for chromatographic fingerprint of tradition Chinese medicine (Version 2004 A). Results: Fingerprints of 11 batches of HZDP were established and 18 common peaks were identified, 13 of which belonged to herbs and were identified by the reference substance and UFLC-IT-TOF/MS. Among them, five common peaks (peaks 6, 7, 9, 10, and 12) came from Angelicae Dahuricae Radix, three common peaks (peaks 4, 5, and 8) came from Citri Reticulatae Pericarpium, four common peaks (peak 1, 2, 11, and13) came from Magnoliae Officmalis Cortex, and one common peak (peak 17) came from Atractlodis Rhizoma. Conclusion: The method is rapid, accurate, reliable, and reproducible. The established fingerprint could provide the references for the study of substance basis and quality control of HZDP.

Identification and comparative analysis of the major chemical constituents in the extracts of single fuzi herb and fuzi-gancao herb-pair by UFLC-IT-TOF/MS / 中国天然药物

AIM@#The aim of this work was to establish a specific and sensitive method to comprehensively investigate and compare chemical constituents of Fuzi-Gancao herb pair (FG), consisting of Aconitum carmichaelii Debeaux (Fuzi, Chinese) and Roast Radix Glycyrrhizae (Glycyrrhiza glabra L., Gancao, in Chinese) and Fuzi alone to explore the underlying interaction mechanism of FG.@*METHOD@#An ultra-fast liquid chromatography-ion trap/time-of-flight mass spectrometry (UFLC/MS-IT-TOF) method using diazepam as internal standard was developed for the identification and semi-quantitative analysis of the phytochemical constituents of Fuzi and FG. Chromatographic separation was achieved on a UFLC column using a gradient program with 40 mmol·L(-1) ammonium acetate and acetonitrile as the mobile phase.@*RESULTS@#Fifty-one of the sixty compounds, including forty-five C19-diterpenoid alkaloids and six C20-diterpenoid alkaloids were tentatively identified in the extracts of Fuzi and FG through accurate mass measurements and fragmentation patterns. Comparing the contents of these alkaloids in these two extracts, it was found that the diester-diterpenoid alkaloids (DDAs) and the alkylolamine-diterpenoid alkaloids (ADAs) were increased, while the monoester-diterpenoid alkaloids (MDAs) were decreased in the extracts of FG.@*CONCLUSION@#This work provided comprehensive information for the quality control of Fuzi preparations, and the further investigation on the compatibility mechanisms of FG.