RESUMEN
A molecular imprinting polymer technique was successfully applied to precipitation polymerization by using styrene as a functional monomer, curcuminoids as templates, acetonitrile as a porogenic solvent, benzoyl peroxide as the initiator, and ethylene glycol dimethacrylate as the crosslinker. The effects of interaction on the adsorption capacity of the molecularly imprinted polymer (MIP) and non-imprinted polymer (NIP) were investigated. A comparison of the adsorption capacity for MIP and NIP indicated that the NIP had the lowest adsorption capacity. The curcuminoid-imprinted polymer (Cur-MIP) was syn-thesized from 0.0237 mmol of styrene, 47.0 g of acetonitrile, 1.0238 mmol of ethylene glycol dimetha-crylate, 0.0325 mmol of curcuminoids, and 0.2480 mmol of benzoyl peroxide. A high-performance liquid chromatography method with fluorescence detection was developed and validated for various chro-matographic conditions for the determination of the curcuminoids in turmeric samples. The sample solution was separated using the Cur-MIP via solid-phase extraction and analyzed on a Brownlee ana-lytical C18 column (150 mm × 6 mm, 5μm) using an isocratic elution consisting of acetonitrile and 0.1%trichloroacetic acid (40:60, v/v). The flow rate was maintained at 1.5 mL/min. The fluorescence detector was set to monitor atλex = 426 nm andλem = 539 nm. The quantification limit values were found to be 16.66, 66.66, and 33.33μg/L for curcumin, demethoxycurcumin, and bisdemethoxycurcumin, respec-tively. Thus, we concluded that the Cur-MIP and high-performance liquid chromatographic-fluorescence method could be applied to selective extraction and could be used as a rapid tool for the determination of curcuminoids in medicinal herbal extracts.
RESUMEN
Microwave-assisted extraction was optimized with response surface methodology for HPLC-fluorescence determination of puerarin and daidzein in Radix Puerariae thomsonii.The optimized extraction procedure was achieved by soaking the sample with 70% methanol（1∶15,v/v）for 30 min,and then microwave irradiation for 11 min at a power of 600 W.Coupling the extraction process with HPLC-fluorescence presented good recovery,satisfactory precision,and good linear relation.Compared with a method from the Chinese Pharmacopoeia,the proposed method enables higher extraction efficiency and more accurate analytical results.It can be of potential value in quality assessment of Radix Puerariae thomsonii medicinal materials.
RESUMEN
OBJECTIVE:To establish a HPLC-fluorescence detection method for the determiniation of the serum concentration of metoprolol.METHODS:The determination was performed on Symmetry C18 column,and the mobile phase consisted of acetonitrile-water-triethylamine -phosphoric acid(110∶390∶2.5∶1.6) at a flow rate of 0.8 mL?min-1.The excitation wavelength was 265 nm and the emission wavelength 298 nm,and the sample size was 20 ?L.RESULTS:Good linearity was obtained for metoprolol over the range of 2.0～100.0 ?g?L-1 with correlation coefficient r=0.999 6.At low,medium and high concentrations,the average recoveries of metoprolol were 99.73%,98.21% and 99.38%,respectively.The intra-day RSD were 2.89%,2.36% and 1.32%,respectively,and the inter-day RSD were 3.73%,3.03% and 2.25% respectively.The lowest detectable limit was 1.0 ?g?L-1.CONCLUSION:This method is precise,accurate,specific,simple yet with high recovery,and it is applicable for clinical monitoring of blood concentration and pharmacokinetic study.
RESUMEN
AIM: To study the bioequivalence of domestic and imported Metoprolol Tartrate Tablets in Chinese healthy volunteers.METHODS: According to the rule published by SFDA,the serum concentration of 20 selected volunteers among 18 to 40 years old was determined by HPLC-fluorescence detection after giving domestic and imported Metoprolol Tartrate Tablets 0.1g,and the pharmacokinetic parameters were calculated by DAS software.RESULTS: The method of HPLC-fluorescence detection to study the pharmakokinetics of Metoprolol Tartrate was sensitive,reliable,accurate and reasonable.The main pharmakokinetics parameters of domestic and imported Metoprolol Tartrate Tablets were T_(max):(1.11)?(0.36 h) and(1.39)?(0.65 h) respectively;C_(max):(269.20)?(87.15)(?g?L~(-1)) and(262.03)?(75.52)(?g?L~(-1)) respectively;AUC_(0-12h):(1088.91)?(510.52)(?g?L~(-1)?h) and(1098.29)?5(55.14)(?g?L~(-1)?h) respectively.The relative bioavailability of domestic Metoprolol Tartrate Tablets was(100.09)%.CONCLUSION: The domestic and imported Metoprolol Tartrate Tablets was bioequivalents.
RESUMEN
OBJECTIVE:To evaluate the human body pharmacokinetics and bioequiavailability of two kinds of oral single dose of hydrochloric itraconazole capsules.METHODS:A randomized,crossover study of20healthy volunteers receiving sin-gle oral dose of200mg itraconazole was conducted with in vivo blood concentrations determined by HPLC-fluorescence de-tection.RESULTS:The pharmacokinetic parameters for the testing itraconazole and the reference itraconazole were as fol-lows,t 1/2 were(29.3?5.62)h and(29.3?5.81)h,respectively;C max were(81.4?60.0)?g/L and(77.8?45.2)?g/L,respec-tively;t max were(3.9?0.70)h and(4.2?0.70)h,respectively;AUC 0～72 were(1199.4?649.6)(?g?h)/L and(1174.3?701.9)(?g?h)/L,respectively;AUC 0～∞ were(1414.0?815.2)(?g?h)/L and(1386.1?735.8)(?g?h)/L,respectively.there were no significant differences in main pharmacokinetics parameters between2preparations,except in t max from analysis of variance and one-side&two-sides t-tests.The relative bioavailability of trial itraconazole capsule was(105.3?23.4)%.CONCLUSION:These two kinds of itraconazole capsules are bioequivalent.
RESUMEN
OBJECTIVE:To establish a method for the determination of sodium valproiate in human serum and to study the bioequivalence of steady state concentration C ssm in of the domestic and imported sodium valproiate sustained-release compound tablets.METHODS:Two periods of multi-oral administration of domestic and imported sodium valproiate sustained-release compound tablets were conducted alternately at random on20healthy male volunteers;the trough concentration of sodium valproate in human serum was determined by HPLC-fluorescence detection and the data were analyzed by3p97pro?gram.RESULTS:The blood concentration was steady after3d oral administration of both the domestic and imported sodium valproate sustained-release compound tablets.The C ssm in of domestic and imported products were(38.17?9.36)、(35.48?9.44)mg/L respectively.C ss min of domestic and imported sodium valproate sustained-release compound tablets were of bioe?quivalence either single or multi-oral administration.CONCLUSION:This HPLC-fluorescence method is quick,sensitive and economical,which can be used to monitor the concentration of sodium valproate in human serum.