A simple and sensitive high performance liquid chromatography method using fluorescence detection (HPLC- FLD) and a one-step single solvent extraction for the determination of prazosin(PZS) in dog plasma is developed and validated. After extraction with ether, the chromatographic separation of PZS is carried out using a reverse phase C18 column ( 150 mm ×4.6 mm, 5 μm) with a mobile phase of 30% acetonitrile and 70% acetic acid-sodium acetate buffer solution (pH = 3.6) and quantified by fluorescence detection operated with an excitation wavelength of 258 nm and an emission wavelength of 387 nm. The flow rate of the mobile phase is 1.0 mL/min and the retention time of PZS and the internal standard is found to be 4. 4 and 5. 8 rain, respectively. The calibration curve is linear within a concentration range from 1.0 to 1 000.0 ng/mL ( P 〉 0. 998). The limit of detection is 0.4 ng/mL. The inter-day coefficient of variation (COV) of the calibration standards is below 5.0% and the mean accuracy is in the range from 92. 7% to 104. 2%. Moreover, by analyzing quality control plasma samples for three days, the results show that the method is precise and accurate, for the intra- and inter- day COV within 10% and the accuracy from 95.9% to 112.7%. The developed and validated method is successfully applied to phannacokinetic study for the preclinical evaluation of a new peroral PZS-sulfobutyl ether beta-cyclodextrin (PZS-SBE-β-CD) inclusion complex tablets (test preparation), which demonstrates that the test preparation released PZS is conducted in a slow and controlled way, and the relative bioavailability of the test preparation is found to be 105.0%.
In this article, a new method for simultaneous determination of six phthalate esters was developed by a combination of electrospun nylon6 nanofibers mat-based solid phase extraction with high performance liquid chromatography-ultraviolet detector (HPLC-UV). The six phthalate esters were dimethyl phthalate (DMP), diethyl phthalate (DEP), butyl benzyl phthalate (BBP), di-n-butyl phthalate (DBP), di-(2-ethylhexyl) phthalate (DEHP) and dioctyl phthalate (DOP). Under optimized conditions, all target analytes in 50 mL environmental water samples could be completely extracted by 2.5 mg nylon6 nanofibers mat and eluted by 100 μL solvent. Compared with C18 cartridges solid phase extraction, C 18 disks solid phase extraction and national standard method (China), nylon6 nanofibers mat-based solid phase extraction was advantageous in aspects of simple and fast operation, low consumption of extraction materials and organic solvents. The four methods were applied to analysis of environment water samples. All the results indicated that the determination values of target compounds with the proposed method were consistent with C18 cartridges and C18 disks solid phase extraction method, and the new method was better than the national standard method in aspects of recovery, LOD and precision. Therefore, nylon6 nanofibers mat has great potential as a novel material for solid phase extraction.