1.Determination of Eugenol in Dikou Lizhong Wan by HPLC Combined with Solid-Phase Extraction
Traditional Chinese Drug Research & Clinical Pharmacology 2000;0(06):-
Objective: To establish a method for the determination of eugenol in Dikou Lizhong Wan. Methods: The sample was first purified on Sep-Pak C18 microcolumn. The chromatographic conditions were as follow: Kromasil C18 chromatographic column (200mm′4.6mm , i.d. 5mm), methanol-water mixed solution (60 ∶40) as mobile phase , the detection wavelength at 270 nm and the flow rate being 1.0 mL?min-1. Results: The average recovery of eugenol was 99.0 %and RSD= 1.8 %(N=6). Conclusion: This method was simple, convenient, rapid,accurate and reliable and it can be used to control the quality of Dikou Lizhong Wan.
2.COMPARATIVE STUDIES ON SEVERAL BIOCHEMICAL INDICES OF ANOPHELES ANTHROPOPHAGUS AND ANOPHELES SIN ENSIS
Chinese Journal of Parasitology and Parasitic Diseases 1987;0(04):-
Proteins, sugars and esterase isoenzymes of An. anthropophagus and An. sinensis were compared by IEF and two dimensional gel electrophoresis.The results show that there are some differences in the electrophoretic patterns between An. anthropophagus and An. sinensis. The glycoprotein, lipidprotein, glycolipi-dprotein, protein, polysaccharide and esterase isosnzymES showed 10, O, 6, 14, 2 and 13 bands in An. anthropophagus; 10, l, 5, 16, 3 and 15 in An. sinensis. There exist 234 and 240 polypeptide spots in An. anthropophagus and in An. sinensis, respectively, alto-gether 27.8% of polypeptide spots being different.
3.Identification of Testosterone and Methyltestosterone in Cosmetics by HPLC-MS
Ximei WU ; Jiemin ZHU ; Binghui ZHU
Journal of Environment and Health 1989;0(06):-
Objective To establish an LC-MS method for identification of testosterone and methyltestosterone in cosmetic.Methods Testosterone and methyltestosterone in cosmetic were determined by liquid chromatography mass spectrometry system which can incorporate electrospray ionization interface,post-column addition agent of formic acid.Results The condition of determination was investigated and optimized.The structure of testosterone and methyltestosterone were identified by direct comparison of the observed mass spectra or by the characteristic ions in the selected-ion monitoring as well as MS2 mode.A doubtful testosterone positive cosmetic was identified by this method,it was negative.Conclusion This method has a high sensitivity and a good reproducibility.It is proved that the method is especially suitable for detection of testosterone and methyltestosterone in cosmetics.
4.Determination of Hesperidin in Xiangsha Yangwei Pill by HPLC
Jialin FANG ; Binghui ZHU ; Jihu FANG
Traditional Chinese Drug Research & Clinical Pharmacology 1993;0(03):-
Objective To establish a method for the determi nation of hesperidin in Xiangsha Yangwei Pill(XYP).Methods Reversed -phrase HPLC was adopted.T he sample was injected into Sep -Pak C 18 cartridge for sample purifica-tion.The chromatographic conditio ns were:Prodigy ODS(150mm?4.6mm,5?m)as analytic column,methanol -wa-ter -acetic acid(35:61:4)as mobile phase,detect wavelength a t 283nmand the flowrate being 1.0mL /min.Results The linear range of hesperidin was from0.148~1.481?g,r =0.9998.The mean recovery was 100.3%,RSD =1.5%(n=6).Conclusion This method was simple,practical,accurate and suitable for the qualit y control of XYP.
5.Determination of forsythin in Shuanghuanglian Oral Liquid by RP-HPLC
Yong CHEN ; Binghui ZHU ; Jihui FANG ;
Chinese Traditional Patent Medicine 1992;0(10):-
Objective: To establish a method for determination of forsythin in Shuanghuanglian Oral (Flos Lonicerae, Radix Scutellariae, Fructus Forsythiae, etc.) Methods: After processing by RP SPE (reverse phase solid phase extraction), the sample solution was measured by RP HPLC. The chromatographic conditions were: Prodigy ODS (3) (150?4.6mm,5?m) column as analytic column; MeOH H 2O HAc(40∶60∶1,V/V) as mobile phase; detection wavelength at 227nm; column temperature at 35?C ; flow rate at 1.0mL?min -1 . Results: The linear range of forsythin was 0.1~2.0?g, r =0.9997. The average recovery was 102.2%, RSD =0.61%( n =6). Conclusion: The method is simple, accurate, reproducible and can be used to enhance the quality control of this drug.
6.Ultrastructural Changes in the Midgut Epithelium of Ixodes sinensis after Infesting the Rabbits Immunized by Purified Ixodic Protein
Zhigang LIU ; Binghui YE ; Qingxian ZHU
Chinese Journal of Parasitology and Parasitic Diseases 1987;0(01):-
Objective To observe the ultrastructural changes in the midgut epithelium of Ixodes sinensis after infesting rabbits immunized with {Mr 105 000} purified tick antigen. MethodsNew Zealand rabbits were inoculated with {Mr 105 000} purified antigen by means of mutiple intradermal injection in foot pad, groin and back. Each immunized rabbit was infested by 30 female Ixodes sinensis. At 24 hours, 48 hours, 72 hours, 5 days and 8 days after infestation, three Ixodes sinensis in each group were observed for ultrastructural changes in the epithelium of their midgut. Results Histological examinations showed that with the time going, digestive cells of the ticks after infesting hosts became more and larger with dense and regularly arranged microvilli, enriched organella, distinct unit_membrane structure, and the appearance of tubli, small vacuole, numerous lipid droplets and hematin granules. These cells also developed a highly infolded basal lamina, forming a labyrinth system. The digestive cells of immunized group were however greatly damaged, whose number and volume were significantly different from control groups. From 24 to 48 hours after infestation, the midgut epithelium of Ixodes sinensis showed pathological changes with the basal lamina becoming thinner, looser and broken; digestive cells damaged and vacuolated; microvilli decreased, shortened and irregularly arranged; the mitochondria swollen and its crests reduced, shortened and even with myeloid changes; the rough endoplasmic reticulum dilated; lipid droplets and hematin granules decreased; phagocytic and pinocytic activity weakened; and basal labyrinth system vacuolated. From 72 hours to 8 days after infestation, cells were severely damaged, organella were denatured and necrotic, nuclei showed pyknosis and cells lysed. Conclusion The rabbits immunized with {Mr 105 000} purified ixodic protein have acquired the adoptive immunity against Ixodes sinensis; in the anti_tick immunity described above, the midgut of Ixodes sinensis is the major affected site.
7.HPLC Determination of Baicalin in Jian' er Xiaosi Oral Liquid
Jinfei LI ; Binghui ZHU ; Yang LI
Traditional Chinese Drug Research & Clinical Pharmacology 1993;0(03):-
Objective To establish a method for the content determination of baicalin in Jian' er Xiaosi Oral Liquid.Method A HPLC method was adopted.The chromatography conditions were as follows:Prodigy ODS(150 mm? 4.6 mm,5 ? m)served as stationary phase and methanol-water-glacial acetic acid(v/v,47:53:1.5)as mobile phase,the detection wavelength was 280 nm,column temperature 35 ℃ and flow rate 1.2 mL/min.Results The amount of inlet baicalin had a good linearity with the response value of peak area in the range of 0.284~ 3.540 ? g,r=0.999 9.The average recovery of baicalin was 100.33 % and RSD was 0.58 %(n=6).Conclusion This method is simple,rapid,reliable,reproducible,and can be used for the quality control of Jian' er Xiaosi Oral Liquid.
8.Determination of Puerarin in Some Chinese Patent Medicines Containing Radix Purerariae by SPE- HPLC
Jihui FANG ; Binghui ZHU ; Yuting ZOU ; Jinxiong YU
Traditional Chinese Drug Research & Clinical Pharmacology 1993;0(03):-
Objective To established a method for the determination of puerarin. Method The sample solutions were pretreated by solid phase extraction (SPE): the specimens were eluted and the cartridges saturated gradually by them in the SPE, but the strongly absorbed impurities were held by the cartridges all the same, and then the effluents were measured by HPLC. Results The linear range of puerarin was 0.205~ 2.464? g, r=0.9999. The average recovery of puerarin in Xintong Oral Liquid, Radix Purerariae and Ganmao Zhike Capsule were 99.5 % , 99.9 % and 98.5 % , RSD were 1.67 % , 1.45 % and 0.95 % (n=5) respectively. Conclusion The method is simple and accurate and can be used for the determination of puerarin in the Chinese patent medicines containing Radix Purerariae.
9.Determination of Metamizole Sodium and Chlorphenamine Maleate in Zhongganling Tablets by Solid-Phase Extracting HPLC
Yiying LIANG ; Binghui ZHU ; Huiwen LU ; Jinxiong YU ; Zhihua DENG ;
Chinese Traditional Patent Medicine 1992;0(04):-
Objective: To establish a method for the determination of metamizole sodium and chlorphenamine malete in zhongganling Tablets. Methods: The sample was determined by ion pair HPLC after it was purified on Sep Pak C 18 microcolumn. The chromatographic conditions included: Hypersil DBS C 18 chromatographic column (250mm?4.6mm, i.d.5?m) as an anlaytical column, methanol mixed solution of sodium heptanesulfonate and glacial acetic acid (600∶400) as a mobile phase, the detection wavelength at 264nm and 1.0mL?min -1 of flow rate. Results: The average recoveries of metamizole sodium and chlorphenamine maleate were 99.6% (RSD was 2.1% and n was 6) and 98.0% (RSD was 1.5% and n was 6), respectively. Conclusion: Metamizole sodium and chlorphenamine maleate can be determined respectively by HPLC with the same mobile phase when Sep Pak C 18 microcolumn solid phase extraction method is used to substitute for the traditional sample pretreatment methods refluxing, extracting and concentrating, and sodium heptanesulfonate ion pair reagent in acid condition is selected.
10.Determination of taurocholic acid in Shedanchuanbei Oral Liquid and snake bile by SPE-HPLC
Binghui ZHU ; Jihui FANG ; Jinfei LI ; Huanguang CHEN ; Huiwen LU ;
Chinese Traditional Patent Medicine 1992;0(04):-
Objective: To establish the method for determination of taurocholic acid in the Traditional Chinese Medicine Shedanchuanbei Oral Liquid and snake bile. Methods: The sample was prepared as mixed solution containing methanol and KH 2PO 4. The mixed solution was injected into Sep Pak C 18 cartridge for the purpose of sample purity. In this processing, the substances which having strong retain action and could harm analytic column were hold in the Sep Pak C 18 cartridge. The eluting solution that the Sep Pak C 18 cartridge had be over loading for taurocholic acid was used as the test solution. The test solution was measured by RP HPLC. The chromatographic conditions were as followed: Supelcosil LC 8 column(150mm?4.6nm,5?m) as analytic column, detect wavelength at 203nm, and MeOH 0.4%KH 2PO 4 mixed solution(56∶44, V/V ) as mobile phase. The inject volume was 50?L. Results: The linear response range of sodium taurocholate was from 0.0253mg?mL -1 to 0.253mg?mL -1 , and the correlation coefficient was 0.9999. The average recovery rate was 101.3%, RSD was 0.40%( n =6). Conclusion: This method was simple, efficient and suitable to the quality control for Shedanchuanbei Oral Liquid and snake bile.