A homologues prediction strategy for comprehensive screening and characterization of C21 steroids from Xiao-ai-ping injection by using ultra high performance liquid chromatography coupled with high resolution hybrid quadrupole-orbitrap mass spectrometry.

Because of the complicated chemical composition of Traditional Chinese Medicines, their chemical profile study has been a great challenge. In the present work, a homologues prediction strategy for rapid screening and identification of C21 steroids in Xiao-ai-ping injection was developed by using an ultra high performance liquid chromatography coupled with high resolution hybrid quadrupole-orbitrap mass spectrometry. This strategy was characterized by the design of C21 steroidal skeleton, substituent group and glycan chain in an orderly way, which could quickly and efficiently screen the interested precursor ions. As a result, a total of 95C21 steroids including 47 potential new ones were identified or tentatively identified, which greatly expanded our knowledge of C21 steroids in Xiao-ai-ping injection. The results indicated that the homologues prediction strategy not only provided an efficient technique to screen and identify target constituents, but also offered a new perspective for discovery new components in Traditional Chinese Medicines.

Chemical profiling and quantification of Dan-Deng-Tong-Nao-capsule using ultra high performance liquid chromatography coupled with high resolution hybrid quadruple-orbitrap mass spectrometry.

Dan-Deng-Tong-Nao capsule (DDTN) was a traditional Chinese medicine (TCM) formula, and has been widely used for the treatment of stroke clinically which caused by blood stasis. However, the bioactive substances and mechanism are unclear because of the complex compositions in DDTN. In this research, An ultra high-performance liquid chromatography (UHPLC) coupled with hybrid quadruple-orbitrap mass spectrometry (Q-Orbitrap MS) method was utilized to identify the chemical constituents of DDTN. In total, 102 compounds including diterpenes, lactones, flavonoids, and phenolic acids were identified by the accurate masses and fragmentation pathways, and 18 of them were unambiguously determined by comparison of reference standards. Besides, 12 representative compounds were simultaneously quantification analyzed and successfully applified for detecting in 9 batches of DDTN samples by UHPLC-Q-Orbitrap MS in parallel reaction monitoring (PRM) mode. The proposed approach was validated to be satisfied in terms of linearity (0.9954-0.9999), LOD (0.771ng/mL), LOQ (2.568ng/mL), intra-day precision ( <2.68%), inter-day precision ( <4.52%), repeatability ( <2.96%), stability ( <3.21%), and recovery (94.6-105.5%). The results indicate that the method of combining UHPLC with Q-Orbitrap MS is practical and efficient for the chemical clarification in DDTN, and has great potential for the integrating quality control of other traditional Chinese medicines.

Antiviral Triterpenes from the Twigs and Leaves of Lyonia ovalifolia.

Eleven new 9,10-seco-cycloartan triterpene glycosides (1-11), seven new lanostane triterpene glycosides (12-18), and two new ursane triterpenoids (19-20) were isolated from the twigs and leaves of Lyonia ovalifolia. The structures of these compounds were elucidated by extensive MS and NMR spectroscopic analysis. The absolute configuration of compound 1a (the aglycone of 1) was established by X-ray crystallography, and that of C-24 in compounds 2, 7, and 12 was established by Mo2(OAc)4-induced electronic circular dichroism experiments. All compounds were evaluated for their antiviral [herpes simplex virus-1 (HSV-1), influenza A/95-359 (A/95-359), and Coxsackie B3 (CVB3)] activity. Compounds 1, 1a, 2a, 12a, 13, and 16 exhibited potent activity against HSV-1, with IC50 values from 2.1 to 14.3 µM, while compounds 1a, 2a, 12a, 13, and 12-2a exhibited potent activity against A/95-359, with IC50 values from 2.1 to 11.1 µM. In turn, compounds 1, 1a, 2a, 12a, and 13 exhibited potent activity against CVB3, with IC50 values from 2.1 to 11.1 µM.