Chemical constituents from Piper wallichii

Fifteen known compounds including four triterpenoids (1–4), one sterol (5), one diketopiperazine alkaloid (6) and nine phenolics (7–15) were isolated from the stems of Piper wallichii. Their structures were elucidated by means of spectroscopic analysis, and acidic hydrolysis in case of the 2-oxo-3β,19α,23-trihydroxyurs-12-en-28-oic acid β-D-glucopyranosyl ester (1). The structure of compound 1 was fully assigned by 1D and 2D NMR experiments for the first time. All isolates were tested for their antibacterial, antifungal, anti-inflammatory and antiplatelet aggregation bioactivities.     

Two new eudesmane-type glucopyranosides from the fruits of Daucus carota L.

Two new eudesmane-type glucopyranosides have been isolated from the fruits of Daucus carota L. On the basis of their spectroscopic and chemical evidence, the new compounds were elucidated as daucucarotol-10-O-β-d-glucopyranoside (1) and decahydro-7-[(2-O-β-d-glucopyranosyl)-isopropyl]-1β,4aα-dimethyl-(1α,4α,8aβ)-naphthalenetriol (2). Compounds 1 and 2 showed moderate antitumour activity against human ECA-109 and gave IC₅₀ values of 23.22 and 26.76 μM, respectively.     

Unprecedented C_(19)-diterpenoid alkaloid glycosides from an aqueous extract of “fu zi”: Neoline 14-O-L-arabinosides with four isomeric L-anabinosyls

Four structurally unprecedented aconitane-type C_(19)-diterpenoid alkaloid glycosides with isomeric arabinosyls, named aconicarmichosides A–D(1–4), were isolated from an aqueous extract of "fu zi", the lateral roots of Aconitum carmichaelii. Their structures were determined as neoline 14-O-a-and 14-O-b-L-arabinopyranosides(1 and 2) and 14-O-a-and 14-O-b-L-arabinofuranosides(3 and 4), by spectroscopic and chemical methods including 2D NMR experiments and acid hydrolysis. Compounds 1–4 represent the first examples of glycosidic diterpenoid alkaloids.     

Direct analysis of anabolic steroids in urine using Leidenfrost phenomenon assisted thermal desorption-dielectric barrier discharge ionization mass spectrometry

Rapid detection of trace level anabolic steroids in urine is highly desirable to monitor the consumption of performance enhancing anabolic steroids by athletes. The present article describes a novel strategy for identifying the trace anabolic steroids in urine using Leidenfrost phenomenon assisted thermal desorption (LPTD) coupled to dielectric barrier discharge (DBD) ionization mass spectrometry. Using this method the steroid molecules are enriched within a liquid droplet during the thermal desorption process and desorbed all-together at the last moment of droplet evaporation in a short time domain. The desorbed molecules were ionized using a dielectric barrier discharge ion-source in front of the mass spectrometer inlet at open atmosphere. This process facilitates the sensitivity enhancement with several orders of magnitude compared to the thermal desorption at a lower temperature. The limits of detection (LODs) of various steroid molecules were found to be in the range of 0.05–0.1 ng mL⁻¹ for standard solutions and around two orders of magnitude higher for synthetic urine samples. The detection limits of urinary anabolic steroids could be lowered by using a simple and rapid dichloromethane extraction technique. The analytical figures of merit of this technique were evaluated at open atmosphere using suitable internal standards. The technique is simple and rapid for high sensitivity and high throughput screening of anabolic steroids in urine.     

Analytical methods for anti-doping control in sport: anabolic steroids with 4,9,11-triene structure in urine

Doping control in sport is mandatory to detect and to control the use of prohibited substances. Due to the growing number of targets, the analysis of doping compounds and their metabolites is carried out using established screening methods. However, detection of anabolic steroids with 4,9,11-triene structure in urine is problematic, so it is necessary to improve the methods.We review the state of the art in doping-control analysis of 4,9,11-trien-3-one steroids, providing an overview of the screening and confirmatory methods developed for these analytes in human urine. First, we review chromatographic techniques. We discuss difficulties in the derivatization of those compounds prior to gas chromatography analyses. In recent years, liquid chromatography has been the preferred technique in drug testing in sport, due to the reduced sample pre-treatment, improved limits of detection and comprehensiveness. We also report on advances and limitations of immunochemical techniques for the analysis of this group of substances.     

Separation of saponins and determination of quinovic acid 3-O-α-L-rhamnopyranoside fromNauclea diderrichii (de Wild) Merr. Bark by high performance liquid chromatography

Summary A reversed-phase HPLC determination of 11 saponins and an alkaloid glycoside inNauclea diderrichii bark is described. Quantitative analysis of quinovic acid 3-0-α-L-rhamnopyranoside which is one of the main saponins was determined, using Chrysanthelline A as internal standard. The complete separation was achieved in 47 minutes. The method of quantification was validated.     

一种新的测定一维同核全相关的NMR技术

提出一种新的基于MDY混合脉冲的可测定一维同核全相关的核磁共振技术.称为一维自旋回波MDY相干转移(lD-SEMDY)实验.结果表明.它具有下列突出优点:一是不用Z-滤波技术就可以得到纯吸收型的一维全相关谱(lD-TOCSY).与同类技术相比,操作简便.可节省测定时间.应用范围较广;二是所测定亚谱中的信号归属通过改变混合时间和延迟时间可以得到确定;三是相干转移非常有效.远程磁化转移信号的灵敏度比较高,对弱偶合的自旋体系也可进行测定.以甙类化合物为例讨论了它在谱峰高度重叠的有机结构测定中的应用.     

A New Flavanone and a New Flavanone Glycoside from ScuteUaria baicalensis

A new flavanone （2S）-5, 7, 2＇, 5＇-tetrahydroxy-flavanone 1 together with a new flavanone glycoside （2S）-5, 7, 2＇, 5＇-tetrahydroxy-flavanone 7-O-13-D-glucopyranoside 2, were isolated from the dry roots of Scutellaria baicalensis. Their structures were elucidated on the basis of spectroscopic data.     

An Efficient Way for Glycosylation of Spirostanol

Using thioglycosides as donors, trimethylsilyl trifluoromethanesulfonate (TMSOTf) and N-iodosuccinimide(NIS) as promoter, a modified procedure for the glycosylation of spirostanol was developed. A series of saponins were synthesized in mild condition with excellent yields.