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A novel method for simultaneous determination of 3 rat poisons ( tetramine, bromadiolone, brodifacoum) and 5 toxic alkaloids ( hyoscyamine, scopolamine, gelsemine, strychnine, brucine ) in toxic samples by dispersive liquid-liquid micro-extraction ( DLLME ) coupled with gas chromatography-mass spectrometry was established. A mixture extractant containing 100 μL trichloromethane and 600 μL methanol was injected into the prepared sample to form an emulsion and the extraction process was accomplished. After centrifuged at 8000 r/min for 5 min, the settled drop of trichloromethane solvent was transferred to a conical insert within a GC autosampler vessel, and analyzed by GC-MS. Factors affecting extraction efficiency such as the type and volume of extractant, dispersive agent, extraction time, pH value and salt concentration of extraction system were studied. The limits of detection(LODs) were from 0. 003 to 1 μg/L in water sample, urine sample and rice wine sample. LODs were from 0. 002 to 0. 2 μg/kg in rice sample. The recoveries of toxic samples were in the range of 81. 0%-110%. The relative standard deviations( RSDs) were lower than 7%. The proposed method was sensitive, effective, and suitable for the simultaneous determination of toxic alkaloids and rat poisons in food poisoning sample.
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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.
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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.
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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.
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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.
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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.
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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.
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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.
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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.