1.Determination of caffeic acid in leaves of Ipomoea batatas (Simon Ⅰ) by HPLC
Pingsheng XU ; Zhiyong DAI ; Guishan TAN ;
Chinese Traditional and Herbal Drugs 1994;0(01):-
Object To develop a method for the determination of caffeic acid in Simon Ⅰ. Methods An HPLC method was developed. Kromasil C 18 column and methanol acetic acid as mobile phase. Results Linearity was found in the range of 10 33 165 28 ?g/mL, the average recovery was 99 38%, RSD=1 36%(n=6). Conclusion This method is reliable, accurate and suitable for the determination of caffeic acid.
2.Simultaneous Determination of 6 Organic Solvents in Tosufloxacin Tosylate by Headspace GC
Wei ZHANG ; Wenbo LI ; Xiaoyan LI ; Weijiao WANG ; Guishan TAN
China Pharmacy 2017;28(6):847-850
OBJECTIVE:To establish a method for the residual simultaneous determination of methanol,alcohol,dichlorometh-ane,n-hexane,tetrahydrofuran and benzene in tosufloxacin tosylat. METHODS:Headspace GC was performed on the capillary col-umn with 6%cyanopropylphenyl-94%dimethylpolysiloxane(DB-624)as fixative lipid,temperature programmed,the inlet temper-ature was 180 ℃,detector was flame ionization detector with temperature of 300 ℃,carrier gas was high purity N2 at a flow rate of 1.5 mL/min,split ratio was 10:1,headspace equilibrium temperature was 100℃,equilibrium time was 40 min,headspace sam-ple volume was 10 mL,and the headspace sample volume was 1 mL. RESULTS:The linear range was 178.3-1782.7 μg/mL for methanol (r=0.9991),301.2-3012.1 μg/mL for alcohol(r=0.9997),33.81-338.10 μg/mL for dichloromethane(r=0.9993), 18.02-180.22 μg/mL for n-hexane(r=0.9991),43.26-432.58 μg/mL for tetrahydrofuran(r=0.9991)and 0.1268-1.2681 μg/mL for benzene(r=0.9991);limits of quantification were 0.31,3.00,0.67,0.02,0.005,0.10 μg/mL,limits of detection were 0.15, 1.51,0.22,0.01,0.001,0.05 μg/mL;RSD of precision test was no higher than 3.1%;RSDs of methanol and n-hexane in stabili-ty and reproducibility tests were no higher than 5%;recoveries were 93.72%-102.20%(RSD=3.1%,n=9),90.10%-101.79%(RSD=4.0%,n=9),97.07%-103.11%(RSD=2.0%,n=9),92.38%-103.83%(RSD=3.9%,n=9),95.44%-103.62%(RSD=2.8%,n=9),and 94.00%-104.73%(RSD=4.1%,n=9). CONCLUSIONS:The method is rapid,sensitive,accurate,and suitable for the residual determination of methanol,alcohol,dichloromethane,n-hexane,tetrahydrofuran and benzene in tosufloxacin tosylat.
3.Effects of semiconductor laser on proliferation of multidrug-resistant model of human osteosarcoma cell line(R-OS-732)
Daming QIN ; Dahui SUN ; Guishan GU ; Yan TAN
Journal of Jilin University(Medicine Edition) 2006;0(02):-
Objective To explore the effects of semiconductor laser on proliferation of the multidrug-resistant model of human osteosarcoma cell line(ROS-732).Methods Four test groups and one control group were set up.The test groups were divided into A,B,C and D groups according to the irradiation time(output power was 200 mW).The time of laser irradiation of A,B,C and D groups were 5,10,20 and 40 min,repectively.The control group(E) wasn′t treated with laser irradiation.MTT method was used to observe the proliferation of R-OS-732,and the morphological changes of the cells were observed by inverted microscope.Results The survival rates of cells in all test groups under condition of semiconductor laser irradiation with 200 mW output power and 532 nm weavlength,compared with control group(P
4.Study on inhibitory effect of reinioside C on asymmetric dimethylanginine-induced soluble interacellular adhesion molecule-1 expression and its mechanisms
Qiongmei FU ; Yongping BAI ; Ruizheng SHI ; Jia CHEN ; Yuanjian LI ; Guishan TAN ; Tianlun YANG ; Guogang ZHANG
Chinese Journal of Geriatrics 2009;28(1):66-69
Objective To investigate the inhibitory effect of reiniosidc C (RC) on asymmetric dimethylarginine (ADMA)-induced soluble interacellular adhesion molecule-1 (slCAM-1) expression and its mechanisms. Methods Human umbical vein endothelial cells (HUVEC 12) were cultured.The level of slCAM-1 in the conditioned medium was determined by ELISA. Changes in intracellular reactive oxygen species (ROS) levels were determined by measuring the oxidative conversion of cell permeable 2', 7'-dichlorofluorescein diacetate (DCFH-DA) to fluorescent dichlorofluorescein (DCF) in fluorospectro- photometer, and the nuclear factor-κB (NF-κB) DNA-binding activity was determined by electrophoretic mobility shift assays (EMSA). Results sICAM 1 expressions [(138.02±16.40), (194.52±11.14), (274.28±13.11)ng/L]and the generation of ROS[(75.64±5.22),(100.18±11.15),(107.23±13.45)units] in HUVEC-12 were time dependently increased by ADMA (30 μmol/L). Furthermore, thc generation of ROS [(85.33±8.68), (70.69±7.65),(59.12±4.15)units], activation of NF-κB activity and expression of sICAM-1 [(336.58±23.32),(203.27±25.18) ,(174.13±14.53)ng/L] induced by ADMA were inhibited by reinioside C (1,3,10μmol/L) in a dose-dependent manner. This effect was found to be the same by L-arginine (0.5 mmol/L) as NOS substrate and by pyrrolidine dithiocarbamate (PDTC) (10 μmol/L)as inhibitor of NF-κB.Conclusions Reinioside C attenuates the increase of sICAM-1 induced by exogenous ADMA
5.Determination of six active components in three species of genus Swertia by HPLC multiwavelength with detection.
Kangping XU ; Jian SHEN ; Fushuang LI ; Jianfeng LIU ; Guoru LIU ; Jianbing TAN ; Guishan TAN
China Journal of Chinese Materia Medica 2009;34(11):1384-1389
OBJECTIVETo develop an HPLC method for the quantification of six active components in three species (Swertia davidi, S. nervosa and S. mussotii) .
METHODThe determination was performed on a Hypersil BDS colunm (4. 6 mm x 200 mm, 5 microm). Acetonitrile and 0.5% phosphoric acid solution were used as the mobile phases with a gradient elution. The flow rate was 1.0 mL x min(-1). The UV detection wavelength was at 240, 274, 325 and 334 nm. The column oven temperature was at 25 degrees C.
RESULTSix components were separated commendably in 60 minutes. The calibration curves of swertiamarin, gentiopicroside, norswertianolin, swertianolin, demethylbellidifolin and bellidifolin were in good linearity over the range of 0.520-20.8, 0.202-8.06, 0.107-4.28, 0.097-3.86, 0.094-3.77, 0.101-4.02 microg, respectively (r = 0.999 9). The average recoveries were 98.7%, 98.1%, 98.3%, 98.8%, 98.1% and 98.6%, respectively, and the RSD were less than 3.0% (n = 6).
CONCLUSIONThe method is accurate,simple and reproducible, and can be used to control the quality of Swertia.
Chromatography, High Pressure Liquid ; instrumentation ; methods ; Drugs, Chinese Herbal ; analysis ; Glucosides ; analysis ; Iridoid Glucosides ; Iridoids ; analysis ; Pyrones ; analysis ; Swertia ; chemistry ; Xanthones ; analysis