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OBJECTIVE:To establish a method for the content determination of Esomeprazole sodium for injection. METH-ODS:UPLC-MS/MS was performed. The column of ZORBAX Eclipse Plus C18 with 0.1% formic acid-methanol(73∶27,V/V)at a flow rate of 0.3 ml/min,column temperature was 35℃,analysis time was 5 min,injection volume was 2μl;ionization mode was positive ion mode,ion source temperature was 150 ℃,capillary voltage was 3.0 kV,cone voltage was 50 V,cone flow was 150 L/Hr,desolvation temperature was 450 ℃,desolvation gas flow was 900 L/Hr,nebuliser pressure was 7.0 Bar,parent ion scan range was 100-800 mz/mz,working mode was multiple reaction monitoring mode. RESULTS:The linear range of esomeprazole was 0.2-20.0 ng/ml(r=0.999 7);the limit of quantitation was 50 pg/ml;RSDs of precision,stability and reproducibility tests were lower than 2%;recovery was 99.93%-100.05%(RSD=0.1%,n=9). CONCLUSIONS:The method is simple and accurate,and can be used for content determination of Esomeprazole sodium for injection.
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AIM: To explore a relative quantitative method by establishing HPLC digitized fingerprints of Fructus Gardeniae and taking the control medicinal material as a reference substance. METHODS: The chromatographic fingerprints were obtained by injecting the sample solution each time on a CenturySIL C_(18) BDS column (20 cm?4.6 mm,5 ?m) with the gradient elution solvent system composed of 1% acetate acid-water and 1% acetate acid-acetonitrile.The flow rate was 1.0 mL/min,the column temperature was maintained at(30?0.15) ℃ and the detection wavelength was set at 265 nm.The HPLC fingerprints of the control medicinal material for Fructus Gardeniae were obtained under different injection volumes and calculated by "the digitized evaluation system of the traditional Chinese medicine fingerprint with the super-information characteristics".Equivalent regression curves were obained by making linear regression between the fingerprint peak areas and apparent injection amounts.(RESULTS:) 35 co-possessing peaks were selected as the fingerprint peaks of Fructus Gardeniae by taking Geniposide peak as the reference peak.Both the equivalent relation between each of the ten places and control medicinal material of Fructus Gardeniae and the equivalent relation between each fingerprint peak of different places and that of Fructus Gardeniae control medicinal material were calculated by equivalent regression curves. CONCLUSION: This method can be useful in the quality control of Fructus Gardeniae.It is also of importantance in deeply studying the relative amounts of single fingerprint peak,and it provides reference value in extending the quantitative evaluation methods of TCM.
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AIM:To establish a HPLC diagitized fingerprint for Ixeris sonchifolia Hance Injection to serve as a digitized method criteria for its overall quality control. METHODS: The chromatographic fingerprints were obtained by injecting 20 ?L of the sample solution each time on a Century SIL BDS column (250 mm?4.6 mm, 5 ?m) with the gradient elution solvent system composed of 1% acetic acid water and 1% acetic acid acetonitrile. The flow rate was 1 mL/min, the column temperature was maintained at (30?0.15)℃ and the detection wavelength was set at 265 nm. The chromatographic fingerprints were charateristically digitized and evaluated by the software of the digitized evaluation system of traditional Chinese medicine fingerprint with the super information characteristics to give the 42 parameters such as chromatographic fingerprint index (F), chromatographic fingerprint resolution index (RF), which could thoroughly disclose the hidden information in the fingerprints. Meanwhile, the apparent molecular weight, the peak position, the elution fore index and the pseudo peak area were marked in terms of the principle of QSPR when the two peaks were selected as the reference peaks. RESULTS: 21 co-possessing peaks were selected as the fingerprint peaks of Ixeris sonchifolia Hance Injection by taking caffeic acid peak as the reference peak to establish the digitized fingerprint and obtain the important digital information about its quanlity control. The stabilities among different batches of samples were evaluated by the dual qualitative and dual quantitative similarity method. CONCLUSION: This new digitized fingerprint method with good precision and reproducibility can be perfectly applied to the quality control over Ixeris sonchifolia Hance Injection. Digitized fingerprint obtained from the dual qualitative and dual quantitative similarity method maybe extend further to assess and control the quanlity of TCM.
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AIM: To establish a novel method for the overall quality control of Fructus Gardeniae by HPLC digitized fingerprint and its normalization. METHODS: The chromatographic fingerprints were obtained by injecting 5 ?L of the sample solution each time on a Century SIL C_ 18 BDS column (20 cm?4.6 mm, 5 ?m) with the gradient elution solvent system composed of 1% acetate acid-water and 1% acetate acid- acetonitrile. The flow rate was 1.0 mL /min, the column temperature was maintained at (30?0.15)℃ and the detection wavelength was set at 265 nm. The chromatographic fingerprints were evaluated by the digitized parameters, such as the chromatographic fingerprint index (F), quantitative similarity, etc,. The influence of big peak on similarity was elaborated by direction cosines, and its cancellation was achieved by the qualitative similarity of peak area ratio. RESULTS: 35 co-possessing peaks were selected as the fingerprint peaks of Fructus Gardeniae by taking Geniposide peak as the reference peak. The HPLC digitized fingerprint and its normalization were implemented. CONCLUSION: This method with good precision and reproducibility can be useful in the quality control of Fructus Gardeniae.
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AIM: A HPLC fingerprint method for the quality control of Fructus Forsythiae has been established. METHODS: The chromatographic fingerprints were determined by injecting 5 ?L of the sample solution each time on a CentriSIL BDS colunm(20 cm?4.6 mm,5 ?m) with the gradient elution solvent system composed of 1% acetate acid water and 1% acetate acid acetonitrile.The flow rate was 1 mL/min,the colunm temperature was maintained at(30?0.15)℃ and the signals were acquired at 265 nm.The chromatographic fingerprints were also evaluated by the chromatographic fingerprint index(F),information index of chromatographic fingerprint(I).(RESULTS:)30 co-possessing peaks were selected as the fingerprint peaks,the similarities among samples of Fructus Forsythiae come from 10 production places and its standard chromatographic fingerprints were calculated taking coffeic acid peak as the reference peak. CONCLUSION: This method with good characteristics and specificity can be used in the quality control of Fructus Forsythiae.
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AIM: A capillary electrophoresis fingerprints(CEFP) method of Fructus Gardeniae was established to evaluate its quality. METHODS: The background electrolyte(BGE) was 25 mmol/L sodium borate solution containing 10% acetonitrile.The detection wavelength was 228 nm and 24 kV was applied.Fructus Gardeniae was extracted by water and injectded for 15 s(9 cm).Some parameters were used to evaluate the similarities.(RESULTS): 24 co-possessing peaks were selected as the fingerprint peaks of Fructus Gardeniae taking chlorogenic acid peak as the reference peak.The similarities between each of the ten places and the standard CEFP of Fructus Gardeniae were evaluated both qualitatively and quantitatively.The CEFP was also evaluated by the information index(I) and the relative information index(I_r). CONCLUSIONS: The CEFP has acceptable precision,reproducibility and can be used to control the quality of Fructus Gardeniae.
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AIM: To develope a reversed-phase high performance liquid chromatographic method for the quantitative determination of chlorogenic acid and caffeic acid in Shegan Kangbingdu Injection. METHODS: The operation was carried out in the Kromasil ODS column with the mobile phase consisting of a mixture of water-methanol-acetonitril aceti acid(95∶10∶5∶2,v/v),in which the flow rate of 1.0 mL/min and UV detection wavelength at 326 nm were set to determine the contents of chlorogenic acid and caffeic acid. RESULTS: There were good linear relations between the concentrations and the peak-areas of chlorogenic acid and caffeic acid.The relative standard deviation of peak areas for chlorogenic acid or caffeic acid were 0.60%,0.32%,respectively.The two kinds of standard solutions were both stable in 16 h(RSD=0.54% for CGA,0.11% for CFA).The average recovery was 100.1%,99.6% for CGA,CFA,repectively.The detectable limit(S/N=3)was 0.012,0.020 mg/L,and the quantitative limit (S/N=10) was 0.037,0.052 mg/L,repectively. CONCLUSION:The method is simple,sensitive,rapid and accurate,and can be used for the quality control of Shegan Kangbingdu Injection