A novel and sensitive HPLC-UV method has been developed for the simultaneous determination of twelve major compounds in Longdan Xiegan Pill.The chemical profile of the twelve compounds,including geniposidic acid(1),geniposide(2),gentiopicroside(3),liquiritin(4),crocin(5),baicalin(6),wogonoside(7),baicalein(8),glycyrrhizic acid(9),wogonin(10),oroxylin A(11)and aristolochic acid A(12),was acquired using high-performance liquid chromatography-diode array detector coupled with an electrospray tandem mass spectrometer(HPLC-DAD-ESI-MS).The analysis was performed on a Dikma Platisil ODS C18 column(250 mm×4.6 mm,5 μm)with a gradient solvent system of acetonitrile-0.1% aqueous formic acid.The validation was carried out and the linearities(r〉0.9996),repeatability(RSD〈1.8%),intra-and inter-day precision(RSD〈1.3%),and recoveries(ranging from 96.6% to 103.4%)were acceptable.The limits of detection(LOD)of these compounds ranged from 0.29 to 4.17 ng.Aristolochic acid A,which is the toxic ingredient,was not detected in all the batches of Longdan Xiegan Pill.Furthermore,hierarchical cluster analysis was used to evaluate the variation of the herbal prescription.The proposed method is simple,effective and suitable for the quality control of this traditional Chinese medicine(TCM).
A new cafferic ester, (+)-2-(1-hydroxyl-4-oxocyclohexyl) ethyl caffeate, was isolated from the 80% ethanol extract of the whole plants of Incarvillea mairei var. granditlora (Wehrhahn) Grierson. The structure of the compound was established by spectroscopic methods.
A rapid method based on rapid resolution liquid chromatography(RRLC) coupled with a diode array detector(DAD) was developed for the simultaneous determination of six major constituents(magnoflorine,jatrorrhizine,coptisine,palmatine,berberine and evodiamine) in traditional Chinese medicine(TCM) Zuo Jin Pill(ZJP).The satisfactory chromatographic separation was carried on an Eclipse Plus C18 column(1.8 μm i.d.,150 mm×4.6 mm) by linear gradient elution with a mobile phase of acetonitrile-acetate buffer.All the calibration curves show good linearity(r2 0.9998).The detection limits and quantification limits ranged in 1.4―12 ng and 4.8―30 ng,respectively.The intra-and inter-day precisions were less than 0.63% with accuracies 98.60%―100.78%,and the recoveries were from 99.45% to 100.46%.Furthermore,hierarchical cluster analysis(HCA) was used to evaluate the variation of the herbal prescription.The results demonstrate that this analytical method is simple,sensitive and reliable for rapidly analyzing six major bioactive compounds in ZJPs and is helpful to comprehensively evaluating the quality of this TCM.
A combined method of high performance liquid chromatograph-elecrtrospray-ionization mass spectrometer(HPLC-ESI-MS/MS) coupled with a photodiode array detector(HPLC-DAD) and principal component analysis(PCA) was applied to the qualitative and quantitative analyses of alkaloids in Cortex Phellodendri(CP) samples, and to the differentiation of two species of CP, Cortex Phellodendri Chinensis(CPC) and Cortex Phellodendri Amurensis(CPA). Twenty-two peaks appeared in the HPLC-MS base peak chromatogram of CP detected by the HPLC-ESI-MS/MS analysis, and the alkaloids were identified according to the MSn data, the known MS fragmentation rules and the literature data. Five alkaloids including berberine, palmatine, jatrorrhizine, phellodendrine and magnoflorine were simultaneously determinated by the HPLC-DAD. Berberine was the primary component in all CP samples, and the contents of berberine and palmatine were exploited to be two critical parameters for effective discrimination between the two species of CP. The average content of berberine in CPC(58.75 mg/g) was higher than that in CPA(9.16 mg/g), while the content of palmatine was less, only 0.25 mg/g in CPC and 4.19 mg/g in CPA. With the use of PCA, samples datasets were separated successfully into two different clusters corresponding to the two species, and berberine, pahnatine, phellodendrine and magnoflorine contribute most to the above mentioned calssifying . The proposed method oroved to be a useful tool in the aualitv control of Chinese herbal medicines.
A new nor-sesquiterpene lactone ainsliatone A (1) was isolated from the aerial parts of Ainsliaeafulvioides. Its structure was established by the basis of spectroscopic methods and single-crystal X-ray diffraction analysis.
Yan WangMing Lu XuHui Zi JinJian Jun FuXiao Jia HuJiang Jiang QinShi Kai YanYun Heng ShenWei Dong Zhang
One new and 16 known compounds were isolated from Abies sibirica. Their structures were assigned mainly on the basis of NMR and MS spectroscopic data. In bioassay for anti-proliferative activity against four human tumor cells, compound 7 exhibited selective anti-proliferative activity against COLO-205 tumor cell with an IC50 value of 0.9 μg/mL.
Gui Rong WangYong Li LiWei Dong ZhangXian Wen YangWen Cong LiuJi YeZhi Jun ZhuHong Chen