ABSTRACT
Objective:To detect 11 kinds of illegally added chemicals in anti-fatigue health foods including sildenafil ,tadalafil, vardenafil , acetildenafil , homosildenafil , hydorxyhomosildenafil , norneosildenafil , aminotadalafil , pseudovardenafil , thioaildenafil and noracetildenafil.Methods:An HPLC-MS/MS method was used with LUNA C18(250 mm ×4.6 mm, 5μm)as the analysis column and triethylamine phosphate , acetonitrile and methanol as the mobile phase with gradient elution at the flow rate of 1ml.min-1 .An ESI+scan and an MS/MS mode were applied .The qualitative and quantitative analysis were carried out by HPLC-MS/MS.Results:Through the detection of 100 batches of samples , 85 batches were only found illegally added chemical substance sildenafil mainly at the concentration of 5-15 mg per granule .Conclusion:The method of HPLC-MS/MS can be used as a powerful screening tool for the rapid drug screening in basic level drug control laboratories to reduce chemical substances illegally added in anti -fatigue health foods .
ABSTRACT
AIM:To put forward three-level design(Box-Behnken design)for fitting response surfaces to optimize the extraction technology of total flavonoids from Hypericum ascyron L.METHODS:Four factors,including temperature,reflux time,concentration of ethanol,ratio of solvent to raw material were used to examine the yield of total flavonoids.Prediction was carried out through comparing the observed and predicted values.RESULTS:The results suggested that ethanol concentration and extraction temperature were two statistically significant factors.The optimum conditions of extraction process consisted of the ratio(mL:g)of solvent to material(13.3:1),ethanol concentration(53.2%),extraction temperature(78.7℃)and extraction time(2.3h).Regression coefficient of binomial fitting complex model was as high as 0.984 6.Bias between observed and predicted values was-4.01%.CONCLUSION:Box-Behnken design is success in optimizing the extaction in close agreement with the predicted values of the mathematic model.
ABSTRACT
AIM:To put forward three-level design(Box-Behnken design) for fitting response surfaces to optimize the extraction technology of total flavonoids from Hypericum ascyron L.METHODS:Four factors,including temperature,reflux time,concentration of ethanol,ratio of solvent to raw material were used to examine the yield of total flavonoids.Prediction was carried out through comparing the observed and predicted values.RESULTS:The results suggested that ethanol concentration and extraction temperature were two statistically significant factors.The optimum conditions of extraction process consisted of the ratio(mL:g)of solvent to material(13.3:1),ethanol concentration(53.2%),extraction temperature(78.7℃)and extraction time(2.3h).Regression coefficient of bino-mial fitting complex model was as high as 0.984 6.Bias between observed and predicted values was -4.01%.CONCLUSION:Box-Behnken design is success in optimizing the extaction in close agreement with the predicted values of the mathematic model.