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Wysłany: Czw 1:04, 17 Mar 2011
Temat postu: HPLC determination of CIBA Vision Eye Drops chryso
HPLC determination of CIBA Vision Eye Drops chrysophanol content
rnl solution, plus 95% ethanol 113lnl, make into a solution containing 75% alcohol, ethanol precipitation the second line, filter, filtrate water bath until no alcohol odor volatile, sodium chloride 3.5 ethyl paraben 0.2g, borneol 0.1g (pre-dissolved with a small amount of ethanol), Xu Changqing distillates 45rnl (the equivalent of Cynanchum paniculatum 10g), add distilled water to nearly 500ml, measured pH = 3.66, with 25% sodium hydroxide to adjust pH to 6.36 and continue to add water to 500ml, CIBA Vision eye drops have a negative control solution. 3.4 Preparation of test solution for precision drawing three different batches of CIBA Vision Eye Drops 50fnI, add concentrated hydrochloric acid 5ml, set in boiling water bath heating 30min, immediately cooled, 3 times with ether extraction 100m1 (40.30, 30 a), combined ether solution, naturally evaporated to dryness, residue dissolved in methanol proceeds and set the volume to 1OIT11, was the test solution. 4 Method and system suitability test results were taken 4.1 control solution, test solution, and the negative solution into the chromatograph, record the chromatogram, theoretical plate number was calculated by chrysophanol 7500, the peak chrysophanol and other components the separation> 2, the retention time of about 9min. Negative samples in the peak position chrysophanol no interference peak (see Figure 1), that under the experimental conditions chrysophanol completely separated from other components. 123> 966 942 151 々 Figure 1 CIBA Vision Eye Drops negative solution absorption spectrum curve of the standard 4.2, respectively 3,6,12,18,
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,24,30 g · ml. The reference solution of the sample 20l, record the peak area (see Figure 2). A peak area to chrysophanol for the longitudinal coordinates, chrysophanol concentration C (g · rnl.) As abscissa, regression analysis, the regression equation: A = A 13.9153 +55.3868 C (r = 0.9998) 123> ; 96 c 694 215 for a l2 Figure 2 Absorption spectra chrysophanol standard precision of the preparation of 4.3 3.00, l2.00,
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, 30.00g · ml. Three concentrations of phenol solution of 5 copies of rhubarb by poor. The results in Table 1. Table 1 The precision of the results (a 5) 4.4 recovery test preparation 3.0o, l2.0o, 30.00tLg · Tnl. Three concentrations of phenol solution of 5 copies of rhubarb by Table 2 The repeatability of the recovery test results of 4.5 samples taken 5 copies of the same batch, according to Show that the method is reproducible. Determination of 46 samples of three batches of CIBA Vision eye drops in accordance with the standard method to calculate the concentration of the sample, the results shown in Table 3. · 2O ·> E Figure 3 CIBA Vision Eye Drops for the impurity absorption spectrum 1,2,3 4 chrysophanol sample assay results in Table 3 the sample batch coupling ... (g · Hd) (%) 5 Discussion and Summary CIBA Vision Eye Drops 5.1 Since the interference of other components, by adjusting the ratio of mobile phase, retention time of change chrysophanol so chrysophanol completely separated from other components. 5.2 configuring blank solution, due to the volatile active ingredient Xu Changqing, they must be distilled alone, not together with other herbs to boiling; borneol insoluble in water, adding dissolved with ethanol should be preceded,
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, and then poured into the drug solution, and quickly stir into the same time, to make it quickly dispersed. 5.3 Preparation of test solution,
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, the application of more than 3 times the ether extraction, the extraction liquid when the ether solution and mix well; if extraction times less than normal, the extraction is not complete, measure the phenolic content of the rhubarb is low. Determination of 5.4 to CIBA Vision Eye Drops Chrysophanol Cassia content, simple,
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, fast, sensitive, accurate, reproducible, and can be used as a quality control of the preparation method.
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