ABSTRACT
Objective:To establish a rapid, sensitive and accurate HPLC-QTOF/MS determination method for the illegally added antihypertensive drugs in traditional Chinese medicines and healthy care products .Methods:An Agilent Eclipse plus C 18 column ( 50 mm ×2.1 mm,1.8 μm) was adopted with the mobile phase of 0.5%formic acid and acetonitrile with gradient elution .The flow rate was 0.2 ml· min-1 .The electrospray ionization source was applied and operated in a positive ion mode .Results:The detection limit of 18 antihypertensive drugs was within the range of 0.2-2.5 ng· ml-1 .Reserpine was found in one sample .Conclusion:The method is selective and sensitive , which can be used for the detection of 18 chemical medicines illegally added in antihypertensive traditional Chinese medicines and health care products .
ABSTRACT
Objective:To establish an HS-GC method for the determination of menthol in Xiao ’ er Fufang Mahuangjian Jiegeng syrups. Methods:An Agilent DB-WAX column(30 m × 0. 53 mm,1. 0 μm)with an FID detector was used;the inlet temperature was 150℃, the detector temperature was 250℃;the flow rate of the carrier gas ( N2 ) was 2. 0 ml·min-1 , the split ratio was 1∶1; the headspace equilibrium temperature was 80℃, the balance time was 30 min, and the sample volume was 1ml. Results:The calibration curve of menthol was within the range of 2. 09-20. 92 μg·ml-1, which showed a good linear relationship (r=0. 999 1). The average recovery of menthol was 98. 0%(RSD=1. 8%, n=6). Conclusion: The method is simple, accurate and reproducible, and can be used for the determination of menthol in Xiao’ er Fufang Mahuangjian Jiegeng syrups.
ABSTRACT
Objective:To improve the determination method for the residual solvents in olsalazine sodium. Methods:1,2-Dichlo-roethane and chloroform were determined by headspace GC with a DB-624 capillary column and an FID detector. The column tempera-ture was 110℃. The temperature of the injector and the detector was 200℃ and 250℃, respectively. The carrier gas was nitrogen with a flow of 3. 0 ml·min-1 . The split ratio was 1∶1. Water was used as the solvent. Results:1,2-Dichloroethane and chloroform were completely separated with good linearity within the respective range of 0. 25-2. 52 ( r =0. 999 5 ) and 2. 28-22. 84 μg · ml-1 ( r =0. 999 5). The average recoveries were 98. 4% and 99. 5% with RSD of 1. 14% and 0. 98%(n=9), respectively. The detection lim-it were 0. 02 and 0. 06 μg·ml-1 , respectively. Conclusion:The method is rapid, sensitive and accurate, which can be used in the determination of residual organic solvents in olsalazine sodium.