Method for Analysis and Chemical Confirmation of Sterigmatocystin

1971 ◽  
Vol 54 (1) ◽  
pp. 86-90 ◽  
Author(s):  
Michael Stack ◽  
J V Rodricks

Abstract A method is described for the analysis of grain samples for the presence and quantitative estimation of sterigmatocystin. Initial extraction with acetonitrile-water (9 + 1) containing KCl is followed by partition of the extract first against hexane and then against CHCl3, and, if needed, silica gel column chromatography. This sequence provides an extract in which the sterigmatocystin can be estimated by fluorescence intensity comparison on TLC plates against a pure sterigmatocystin standard. Visualization of the sterigmatocystin on the TLC plates is enhanced by an AlCl3 spray reagent. After preparative TLC, the identity of sterigmatocystin is confirmed by formation of an acetate derivative and of a derivative formed by treating the suspected extract with aqueous acid.

1977 ◽  
Vol 60 (1) ◽  
pp. 104-106
Author(s):  
Albert K Athnasios ◽  
Gustav O Kuhn

Abstract A modified thin layer chromatographic (TLC) method has been developed in conjunction with the method of Stack and Rodricks which effectively separates sterigmatocystin from interfering materials and eliminates the time-consuming column chromatographic cleanup step. Initial extraction with acetonitrile-water (9+1) containing KCl is followed by partition of the extract first against hexane and then against CHCl3. The CHCl3 extract is evaporated and the residue is dissolved in benzene and applied directly to pre-coated high resolution TLC plates, which are developed in benzene-acetic acid (90+10). Visualization of the sterigmatocystin on TLC plates is enhanced by an AlCl3 spray reagent, and concentrations of sterigmatocystin as low as 50 μg/kg can be estimated by comparing fluorescence intensity against a pure sterigmatocystin standard. The method has been applied to barley, white and yellow corn, oats, and wheat. Recoveries of added toxin in the range of 50—400 μg/kg ranged from 86.3% for yellow corn and oats to >96% for barley, wheat, and white corn.


2019 ◽  
Vol 19 (11) ◽  
pp. 1399-1404 ◽  
Author(s):  
Yangcheng Liu ◽  
Wei Liu ◽  
Changlan Chen ◽  
Zheng Xiang ◽  
Hongwei Liu

Background and Purpose:: Patrinia villosa Juss is an important Chinese herbal medicine widely used for thousands of years, but few reports on the ingredients of the herb have been presented. In this study, we aim to isolate the bioactive compound from the plant. Material and Methods:: The air-dried leaves of P. villosa (15kg) were extracted three times with 70% EtOH under reflux. The condensed extract was suspended in H2O and partitioned with light petroleum, dichloromethane and n-BuOH. The dichloromethane portion was then subjected to normal-phase silica gel column chromatography, ODS silica gel column chromatography and semi-preparative HPLC to yield compound 1. Cytotoxicities of 1 were assayed on HepG2, A549 and A2780 cell lines. The mechanism of apoptosis and cell cycle on A549 was confirmed subsequently. Results: A new impecylone (Impecylone A) was isolated from the leaves of Patrinia villosa Juss, and its structures were established using 1D, 2D-NMR spectra and HR-ESI-MS. Impecylone A could selectivity inhibit HepG2 and A549 cell lines. The compound could induce apoptosis of A549 and arrest the cell cycle at G2/M phase in a dose-dependent manner. Conclusion: Impecylone A is a novel compound from Patrinia villosa Juss and could be a potential antitumor agent especially in the cell lines of A549.


1964 ◽  
Vol 5 (3) ◽  
pp. 479-481
Author(s):  
Quincy E. Crider ◽  
Petar Alaupovic ◽  
Joe Hillsberry ◽  
Cathy Yen ◽  
Reagan H. Bradford

2021 ◽  
Vol 22 (14) ◽  
pp. 7482
Author(s):  
Hwan Lee ◽  
Zhiming Liu ◽  
Chi-Su Yoon ◽  
Linsha Dong ◽  
Wonmin Ko ◽  
...  

Aging is associated with immune disregulation and oxidative stress which lead to inflammation and neurodegenerative diseases. We have tried to identify the anti-neuroinflammatory and anti-inflammatory components of Coreopsis lanceolata L. The dried flowers of C. lanceolata were extracted with 70% EtOH, and the obtained extract was divided into CH2Cl2, EtOAc, n-BuOH, and H2O fractions. The CH2Cl2 fraction was separated using silica gel and C-18 column chromatography to yield phenylheptatriyne (1), 2′-hydroxy-3,4,4′-trimethoxychalcone (2), and 4′,7-dimethoxyflavanone (3). Additionally, the EtOAc fraction was subjected to silica gel, C-18, and Sephadex LH-20 column chromatography to yield 8-methoxybutin (4) and leptosidin (5). All the compounds isolated from C. lanceolata inhibited the production of nitric oxide (NO) in LPS-induced BV2 and RAW264.7 cells. In addition, phenylheptatriyne and 4′,7-dimethoxyflavanone reduced the secretion of inflammatory cytokines, tumor necrosis factor alpha (TNF-α), and interleukin (IL)-6. Among them, phenylheptatriyne was significantly downregulated in the expression of inducible NO synthase (iNOS) and cyclooxygenase-2 (COX-2). Subsequently, phenylheptatriyne also effectively inhibited nuclear factor-kappa B (NF-κB) activation in LPS-stimulated BV2 and RAW264.7 cells. Based on these results, the anti-neuroinflammatory effect of phenylheptatriyne isolated from C. lanceolata was confirmed, which may exert a therapeutic effect in treatment of neuroinflammation-related diseases.


ChemInform ◽  
2010 ◽  
Vol 32 (28) ◽  
pp. no-no
Author(s):  
Mikiko Sodeoka ◽  
Ruriko Sampe ◽  
Sachiko Kojima ◽  
Yoshiyasu Baba ◽  
Naoko Morisaki ◽  
...  

1995 ◽  
Vol 144 (3) ◽  
pp. 517-525 ◽  
Author(s):  
S Moslemi ◽  
P Silberzahn ◽  
J-L Gaillard

Abstract Explants of equine full-term placenta have been shown to synthesize 19-norandrogens from labelled androgens. Steroid metabolites were purified by silica-gel column chromatography then analysed and quantified by C18-reverse-phase HPLC coupled to a radioactive flow detector. 19-Norandrostenedione was subsequently recrystallized to constant specific activity, providing unequivocal evidence of its synthesis by the equine placenta. 19-Norandrostenedione synthesis appeared to be localized in the microsomal fraction. Regardless of the substrate used, formation of 19-norandrogens was far weaker than that of oestrogens; moreover, the yield of 17-oxosteroids produced was much greater than that of 17β-hydroxysteroids, suggesting the presence of a dehydrogenase with predominant oxidative activity. Sulphoconjugated steroids formed were less than 0·5% of total steroids. Although 19-nortestosterone could not be generated by equine purified aromatase incubated with labelled testosterone, the synthesis of 19-norandrogens and oestrogens by equine placental explants was blocked by two specific aromatase inhibitors, 4-hydroxyandrostenedione and fadrozole. Our results provide evidence for a placental origin of at least a part of the 19-norandrogens previously identified in the blood of the pregnant mare. Furthermore, it is suggested that 19-norandrogen biosynthesis would involve the enzymatic metabolism of 19-oxygenated androgens formed by equine aromatase. Journal of Endocrinology (1995) 144, 517–525


2021 ◽  
Vol 25 (1) ◽  
pp. 86-92
Author(s):  
B.A. Ayinde ◽  
J.O. Owolabi ◽  
I.S. Uti ◽  
P.C. Ogbeta ◽  
M.I. Choudhary

The antidiarrhoeal effect of Waltheria indica methanol extract and fractions have been reported earlier but, the present work examined the intestinal relaxant effects of two flavonoid-phenyl propanoids isolated from the methanol extract. The active aqueous fraction was subjected to vacuum liquid chromatography using dichloromethane with increasing concentration of ethyl acetate, and that of methanol and water successively. The ten (10) fractions obtained were combined to give seven (7). The fraction 2 (C, D) was subjected to preparative thin layer chromatography on silica gel GF254 (10-40μm) using CHCl3-CH3OH (8:2) to obtain compound coded F2. Fraction 4 (F) was subjected to column chromatography using silica gel (60-120μm mesh) and eluted with  dichloromethane with increasing concentrations of methanol. Fractions 9-28 were combined and subjected to column  chromatography using chloroform with increasing concentration of methanol. The fractions 1-16 of these were purified on Sephadex LH-20 to obtain compound BAA. The identities of the two compounds were established using spectroscopic methods. The  antidiarrheal effect of compound F2 was evaluated on mice using charcoal transit (100,200, 400mg/kg), castor oil (40, 60 mg/kg)  while the two compounds were examined for their inhibitory effects on Ach-induced ileum contraction. The effects of the  compounds were compared with loperamide (3mg/kg) and atropine (80μg). Compounds F2 and BAA were identified as tiliroside and 3’’’, 5’’’-dimethoxy tiliroside respectively. Tiliroside inhibited the charcoal transition in the animals in a dose dependent pattern with 400mg/ mL eliciting 63.41% inhibition compared to 59.23% produced by loperamide. The compound also elicited significantly (P<0.05) prolonged onset of stooling and reduced the number and weight of stools produced lower than the control. The two  compounds drastically inhibited the Ach-induced contractions of the ileum. The compound, tiliroside at 10mg, completely abolished  the contraction by Ach unlike 3’’’, 5’’’-dimethoxy tiliroside which reduced the contraction to 1.92% at 20mg. The identified compounds seem to be responsible for the ethnomedicinal use of the plant in treating diarrhea.


Sign in / Sign up

Export Citation Format

Share Document