We developed and validated a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method to detect and quantitate 14 anti-diabetic, 2 anti-obesity, and 3 cholesterol-lowering drugs in botanical dietary supplements marketed for blood sugar management. Many botanical dietary supplements which carry label statements related to blood sugar management are available over the Internet. Potential adulteration of such dietary supplements with anti-diabetic and other prescription drugs, some of which have been removed from the market due to adverse events, is of concern. No significant matrix effects were observed and mean recoveries of all 19 analytes from a single product matrix were 88 to 113% at spiking concentrations from 500 to 2000 μg/g. Mean recoveries of metformin, phenformin, and sibutramine from matrices prepared from multiple product composites ranged from 93 to 115% at a spiking concentration of 100 μg/g. The relative standard deviations (RSD) (%) of intra-day analyses ranged from 0.2 to 13 for all recovery studies. Eighty dietary supplements obtained in the USA and carrying label statements related to blood sugar management were analyzed using this method and none were found to be adulterated with the above 19 drugs. Two products obtained outside of the USA and known to be adulterated were also analyzed by this method and found to contain phenformin, glibenclamide, and sibutramine. This method provided satisfactory selectivity, linearity, accuracy, precision, and sensitivity for rapid determination of 19 drugs and has broad applicability for the analysis of dietary supplements for possible adulteration with these compounds.
Two new sesquiterpenoid tropolone glycosides, liriosmasides A (1) and B (2), along with two known compounds, secoxyloganin and oplopanpheside C, were isolated from a methanol extract of the roots of Liriosma ovata. The structures of 1 and 2 were elucidated by spectroscopic methods including 1D and 2D NMR and by high-resolution mass spectrometry involving an ultra-high-performance liquid chromatography-quadrupole-orbital ion trap mass spectrometric (UHPLC-Q-Orbitrap MS) method. Compound 1 showed weak inhibitory activity against HIV RNase H.
In this study,Populus deltoides of one year old plant cultivated in some area surrounding Kunming, such as Aziying,Yiliang,Luqian,Xundian,in which have favorable soil condition and thickness of soil have reached 85 -100 cm,were conducted to study the adaptation and flooding tolerance of Populus deltoides planted in Kunming city.The results showed that Populus deltoides planted for three years,survival rate of Populus deltoides in Aziying,Yiliang,Luqian were above 95%,and then growth of average height,of average diameter at breast height and of average canopy on nursery-grown plant were 4.2 m,4 cm,93.6 cm,respectively.Simultaneously,the growth of average height,diameter at breast height and canopy had reached 14 m,13 cm,and 310 cm respectively at place of Aziying,Yiliang,Luqian.Compared with habitat and suitable area,its growing states achieved normal fast-growing level at the three regions.Populus deltoides planted in plots of underground level of 50 cm,100 cm and 150 cm for three years,the average survival rate was about 85%.Among of them,the growth of Populus del-toides was the best in underground water level of 100 cm.It was worse for growth condition of Populus deltoides in coteau plots than in dam beside highway,especially in side of rate of infection diseases and pests,the death rate of branch.Consequently,Populus deltoides should not planted at middle-upper part of coteau.
Increased use of dietary supplements is a phenomenon observed worldwide. In the USA, more than 40% of the population recently reported using complementary and alternative medicines, including botanical dietary supplements. Perceptions that such dietary supplements are natural and safe, may prevent disease, may replace prescription medicines, or may make up for a poor diet, play important roles in their increased use. Toxicity of botanical dietary supplements may result from the presence of naturally occurring toxic constituents or from contamination or adulteration with pharmaceutical agents, heavy metals, mycotoxins, pesticides, or bacteria, misidentification of a plant species in a product, formation of electrophilic metabolites, organ-specific reactions, or botanical-drug interactions. The topics discussed in this review illustrate several issues in recent research on botanical ingredients in dietary supplements. These include (1) whether 1,3-dimethylamylamine is a natural constituent of rose geranium (Pelargonium graveolens), (2) how analysis of the components of dietary supplements containing bitter melon (Momordica charantia) is essential to understanding their potential biological effects, and (3) how evolving methods for in vitro studies on botanical ingredients can contribute to safety evaluations. The virtual explosion in the use of botanical ingredients in hundreds of products presents a considerable challenge to the analytical community, and the need for appropriate methods cannot be overstated. We review recent developments and use of newer and increasingly sensitive methods that can contribute to increasing the safety and quality of botanical ingredients in dietary supplements.
Momordica charantia L. (Cucurbitaceae), commonly known as bitter melon, is widely cultivated in many tropical and subtropical areas of the world. It is a common food staple; its fruits, leaves, seeds, stems, and roots also have a long history of use in traditional medicine. In the United States, dietary supplements labeled as containing bitter melon can be purchased over-the-counter and from Internet suppliers. Currently, no quantitative analytical method is available for monitoring the content of cucurbitane-type triterpenes and triterpene glycosides, the major constituents of bitter melon, in such supplements. We investigated the use of HPLC-electrospray ionization (ESI)-MS/MS for the quantitative determination of such compounds in dietary supplements containing bitter melon. Values for each compound obtained from external calibration were compared with those obtained from the method of standard additions to address matrix effects associated with ESI. In addition, the cucurbitane-type triterpene and triterpene glycoside contents of two dietary supplements determined by the HPLC-ESI-MS/MS method with standard additions were compared with those measured by an HPLC method with evaporative light scattering detection, which was recently developed for quantification of such compounds in dried fruits of M. charantia. The contents of five cucurbitane-type triterpenes and triterpene glycosides in 10 dietary supplements were measured using the HPLC-ESI-MS/MS method with standard additions. The total contents of the five compounds ranged from 17 to 3464 microg/serving.
The antidiabetic activity of Momordica charantia (L.), Cucurbitaceae, a widely-used treatment for diabetes in a number of traditional medicine systems, was investigated in vitro. Antidiabetic activity has been reported for certain saponins isolated from M. charantia. In this study insulin secretion was measured in MIN6 β-cells incubated with an ethanol extract, saponin-rich fraction, and five purified saponins and cucurbitane triterpenoids from M. charantia, 3β,7β,25-trihydroxycucurbita-5,23(E)-dien-19-al (1), momordicine I (2), momordicine II (3), 3-hydroxycucurbita-5,24-dien-19-al-7,23-di-O-β-glucopyranoside (4), and kuguaglycoside G (5). Treatments were compared to incubation with high glucose (27mM) and the insulin secretagogue, glipizide (50μM). At 125μg/ml, an LC–ToF-MS characterized saponin-rich fraction stimulated insulin secretion significantly more than the DMSO vehicle, p=0.02. At concentrations 10 and 25μg/ml, compounds 3 and 5 also significantly stimulated insulin secretion as compared to the vehicle, p≤0.007, and p=0.002, respectively. This is the first report of a saponin-rich fraction, and isolated compounds from M. charantia, stimulating insulin secretion in an in vitro, static incubation assay.
In the paper by Ma et al., Cucurbitane-type triterpenoids from Momordica charantia. Planta Med 2010; 76: 1758– 1761 [1], compound 1 was named momordicoside U (Fig. 1). Unbeknown to the authors, the same name had been given earlier to a different substance in the article by Nguyen et al., Cucurbitane-type triterpene glycosides from the fruits ofMomordica charantia. Magn Reson Chem 2010; 48: 392–396 [2] (compound 1) (Fig. 2). Therefore the compound isolated by Ma et al. is to be renamed “Momordicoside X”. References 1 Ma J, Whittaker P, Keller AC, Mazzola EP, Pawar RS, White KD, Callahan JH, Kennelly EJ, Krynitsky AJ, Rader JI. Cucurbitane-type triterpenoids from Momordica charantia. Planta Med 2010; 76: 1758–1761 2 Nguyen XN, Phan VK, Chau VM, Ninh KB, Nguyen XC, Le MH, Bui HT, Tran HQ, Nguyen HT, Kim YH. Cucurbitane-type triterpene glycosides from the fruits of Momordica charantia. Magn Reson Chem 2010; 48: 392– 396
One new cucurbitane-type triterpenoid glycoside, momordicoside U (1), together with five known cucurbitane-type triterpenoids and related glycosides, 3β,7 β,25-trihydroxycucurbita-5,23 (E)-dien-19-al (2), momordicine I (3), momordicine II (4), 3-hydroxycucurbita-5,24-dien-19-al-7,23-di-O-β-glucopyranoside (5), and kuguaglycoside G (6), were isolated from the whole plant of Momordica charantia. Their structures were determined by chemical and spectroscopic methods. Momordicoside U (1) was evaluated for insulin secretion activity in an in vitro insulin secretion assay and displayed moderate activity.
Polysaccharide was extracted from huhegaridi-9 with hot water-ethanol deposit method and determined by phenol-sulphuric acid method(λ=488nm).The regression equation is y=0.00656x+0.324 and coefficient of correlation r=0.9994.The average recovery is 101.2% with RSD=0.90%(n=5).
The essential oil was extracted from the different zanthoxylum bungeanum by using steam distillation.The amount of the components from the essential oil was determined by monoliration method.The separated main chemical components were identified by TLC and GC-MS.The contents and constituents of these materials from different species or habitats are greatly different.
Pouteria campechiana, Pouteria sapota, and Pouteria viridis are tropical plants in the Sapotaceae family that bear edible fruits. The fresh fruits of these three Pouteria species were each extracted, and activity-guided fractionations were performed to identify the antioxidant constituents. Seven polyphenolic antioxidants, gallic acid (1), (+)-gallocatechin (2), (+)-catechin (3), (-)-epicatechin (4), dihydromyricetin (5), (+)-catechin-3-O-gallate (6), and myricitrin (7), were isolated and identified. Extracts of the three Pouteria fruits were analyzed by a selected ion monitoring liquid chromatography-mass spectrometry method to quantify their polyphenolic antioxidants. The highest level of the seven measured polyphenols was found in P. sapota, the second highest in P. viridis, and the lowest in P. campechiana. The levels of the seven polyphenols corresponded with the results of the 1,1-diphenyl-2-picrylhydrazyl assay, by which P. sapota had the highest antioxidant activity, P. viridis the second highest, and P. campechiana the lowest.
OBJECTIVE To establish a method for the determination of total anthraquinones in Fufang Huangqi tablet. METHODS The detection wavelength of colorimetric methol was 535 nm, the stability of the method was investigated. RESULTS The method is available for quantitative determination of Fufang Huangqi tablets, the content of total anthraquinones per tablet should be controlled (10±1)mg. CONCLUSIONS This method is simple and accurate.
Activity-guided fractionation of a methanol extract from the fruit of Manilkara zapota cv. Tikal resulted in the isolation of two new antioxidants, methyl 4-O-galloylchlorogenate (1) and 4-O-galloylchlorogenic acid (2), along with eight known polyphenolic antioxidants, namely, methyl chlorogenate (3), dihydromyricetin (4), quercitrin (5), myricitrin (6), (+)-catechin (7), (-)-epicatechin (8), (+)-gallocatechin (9), and gallic acid (10). Of the 10 polyphenols, 1 showed the highest antioxidant activity (IC50 = 12.9 muM) in the 1,1-diphenyl-2-picrylhydrazyl (DPPH) free-radical assay and displayed cytotoxicity in the HCT-116 and SW-480 human colon cancer cell lines with IC50 values of 190 and 160 muM, respectively. Compound 2 showed high antioxidant activity (IC50 = 23.5 muM) in the DPPH free-radical assay and displayed cytotoxicity in the HCT-116 and SW-480 human colon cancer cell lines with IC50 values of 154 and 134 muM, respectively.
OBJECTIVE To analyse the chemical constituents from the roots of Glycyrrhiza pallidiflora Max.METHODS The chemical components were obtained by steam distillation,separated and identified by GC MS and elucidated based on the standard mass spectral data respectively.The relative content of each component was calculated by area normalization.RESULTS 25 peaks were separated and all of them were identified.The main chemical components were linoleic acid ethyl ester (32.77%),hexadecanoic acid ethyl ester (10.02%),decane,2,3,7 trimethyl (6.49%),5 methyl heneicosane (5.74%),tricosane (3.80%),1 cyclohexylnonene (3.70%),eicosane (3.63%),octadecanoic acid and ethyl ester (3.59%) respectively.CONCLUSION The study was reported for the first time.The results here provided solid and scientific proof for the further development of Glycyrrhiza pallidiflora Max