OBJECTIVE To establish a HPLC method for simultaneous determination of Mesaconitine,Aconitine and Hypaconitine in blood and liver speciman. METHODS The samples were separated on the column of Welchrom ODS (4.6 mm×250 mm, 5 μm). The mobile phase consisted of acetonitrile-0.03% tetrabutyl ammonium hydroxide (with glacial acetic acid to pH 9.74) (58∶42) at a flow rate of 1.0 mL·min-1 . The detection wavelength was at 230 nm. RESULTS Mesaconitine in biological samples were linear in the ranged of 0.077-23 mg·L-1 (r=0.999 8), and Aconitine was linear in the ranged of 0.083-25 mg·L-1 (r=0.999 8), and Hypaconitine was linear in the range of 0.08-24 mg·L-1 (r=0.999 6). The mean extraction recovery was over 83.6% in biological samples. The intra and inter-day precision of assay for Mspeciman,Aconitine and Hypaconitine were less than 5.1% and 9.3% in biological samples. CONCLUSION The method is simple, sensitive, accurate, and suitable for the determination of Mesaconitine,Aconitine and Hypaconitine in blood and liver speciman for toxicological and clinical pharmaceutical analysis.

OBJECTIVETo establish a new high performance liquid chromatography (HPLC) method for determining the concentration of cefazolin, cefradine, cefoperazone and cefotaxime in blood and urine, as well as to investigate its applicability.METHODSProtein in blood and urine was precipitated directly by acetonitrile with acetanilide was used as the internal standard using Agilent Zorbax SB-Aq column (250 mm x 4.6 mm, 5 microm). The mixed solvents of water (triethylamine 0.12%, acetic acid 0.12%) and acetonitrile were used as the mobile phase to separate cephalosporins using gradient elution method at 1 mL/min (flow rate) and 254 nm (detection wavelength).RESULTSThe working curve of four cephalosporins showed a good correlation (r = 0.9993), with the detection limit up to 0.01 microg/mL. The recovery rate was more than 81.2%.CONCLUSIONThis method is fast, easy and accurate. It is suitable for biological analysis of the 4 cephalosporins of the blood and urine in practical cases.

OBJECTIVE To establish a method for simultaneous determination of Prednisone and Prednisolone in the blood and urine.METHODS The compounds were extracted from blood and urine using ethyl acetate as the solvent for liquid-liquid extraction and detected by HPLC with Betamethasone as the internal standard.Separation was achieved on Zorbax SB-Aq column using methanol-0.01 mol·L-1 potassium dihydrogen phosphate(57:43) as mobile phase.RESULTS The linear limits of Prednisone and Prednisolone ranged from 0.05 μg·ml-1 to 40.00 μg·ml-1 in the blood(r≥0.9997)and 0.04 μg·ml-1 to 50.00 μg·ml-1 in urine(r≥0.9991),respectively.The limits of detection for these two analytes were 0.012 μg·ml-1 and 0.008 μg·ml-1 in the blood and urine,respectively.The intra and inter day assay precision of this method were no more than 7.8%.The mean recovery of Prednisone and Prednisolone in the blood and urine ranged from 92.9% to 106.3%,and the mean extraction recovery of these two analytes was no less than 85.4%.CONCLUSION The method is accurate,sensitive,well reproducible and suitable for simultaneous determination of Prednisone and Prednisolone.

OBJECTIVE:To establish a new method for the analysis of paraquat in blood and urine by sodium borohydride/nickel chloride chemical reduction-gas chromatography/thermionic specific detector.METHODS:An initial procedure of precipitation was performed by adding hydrochloric solution with sodium chloride and a mixture of chloroform and ethanol. Then the analyte contained in supernatant was reduced by a reduction system of sodium borohydride and nickel chloride and extracted by acetic ether. Ethyl paraquat (EPQ) was used as internal standard. GC/TSD was used to identify and quantify the analyte.RESULTS:The limits of detection (S/N=3) in blood and urine were 0.002 and 0.004 microg/mL, respectively. The linear ranges were 0.050-30.0 microg/mL. Correlation coefficients in blood and urine were 0.999 and 0.998, respectively. The recoveries exceeded 80% both in blood and urine.CONCLUSION:This method is applicable for quantification of paraquat in biological fluids.