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Objective:To establish a rapid HPLC testing method for chloroquine phosphate,hydroxychloroquine sulfate and amodiaquine hydrochloride.Methods:The chromatographic separation was performed on a GRACE prevail C18(53 mm×7 mm,3 μm)column,and the column temperature was maintained at 30℃.Acetonitrile-0.3% triethylamine acetonitrile solution (adjusting pH to 3.0 with phosphoric acid) (12∶88) was used as the mobile phase,the flow rate was 1.0 ml· min-1 and the UV detection wavelength was 254 nm.The qualitative research was performed using relative retention time and spectral similarity as the double indicators.The relative correction factor in the quantification analysis was used for the content determination.Results:Three anti-malarial drugs showed good behavior in one chromatographic system.The rapid HPLC testing analysis could be achieved.The qualitative research was more accurate by using the double indicators (UV spectral similarity and relative capacity factor).The HPLC qualitative accuracy was increased.The relative correction factor method for the quantification could effectively reduce the use of reference substances and speed up the analysis of HPLC.Conclusion:The method is rapid and simple,and suitable for the rapid determination of drugs.
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Objective: To establish a content determination method for ferric iron and ferrous iron in ferrous succinate tablets.Methods: Using a Dionex RFICTM protection column (4 mm×50 mm)and a Dionex RFICM Ion PacRCS5A analytical column (4 mm×250 mm), the eluent solution consisted of 7 mmol·L-1 dipicolinic acid, 66 mmol·L-1 potassium hydroxide, 5.6 mmol·L-1 potassium phosphate monobasic and 74 mmol·L-1 formic acid.The flow rate was 1.5 ml·min-1, the column temperature was 30.0℃ and the injection volume was 1.3 μl.Results: Fe3+ showed good linearity within the range of 0.5-15 μg·ml-1(r=1.000 0), Fe2+ showed good linearity within the range of 25-200 μg·ml-1(r=1.000 0), and the average recovery was 103.6%(RSD=2.7%, n=9)and 98.3%(RSD=1.9%, n=9), respectively.Conclusion: The method is simple, reliable and accurate, and can be used for the determination of Fe3+and Fe2+ in ferrous succinate tablets.
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Objective:To establish a method to determine ferrous succinate in ferrous succinate tablets .Methods:Ion chromatog-raphy was performed on an IonPac AG19(4 mm ×250 mm)anion exchange chromatography column with a guard column of Ion Pac TM AG19( 4 mm ×50 mm);30.00 mmol· L-1 KOH was used as the isocratic eluent at a flow rate of 1.00 ml· min-1 with suppressed conductivity detection ( Curb:75 mA) at the temperature of 30℃.The sample size was 25 μl .Results:The linear range of succinic acid was 2.005 1-25.064 0μg· ml-1(r=0.999 5).The detection limit and quantitation limit was 0.12ng and 0.42ng, respectively. The recovery was 101.45%(RSD=0.43%, n=6).Conclusion:The method is simple, rapid, accurate, reproducible and sensitive , and can be used to determine the ferrous succinate content in ferrous succinate tablets .
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OBJECTIVE:To establish a method for the uncertainty measurement evaluation of the content determination of pred-nisolone API. METHODS:HPLC internal standard method was adopted to determine the content of prednisolone API,establish mathematical model for uncertainty evaluation,analyze influential factors and evaluate the factors. RESULTS:HPLC internal stan-dard method showed the contont was 98.8%,and expanded uncertainty of prednisolone API was 1.6%,and the determination result was(98.8±1.6)%,k=2. CONCLUSIONS:The method is suitable for the uncertainty measurement evaluation of the content deter-mination of prednisolone API by HPLC internal standard method.
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Objective: To study the related substances in clozapine and its preparations. Methods:Comparative analysis was adopted according to the method respectively described in Chinese pharmacopoeia and United States pharmacopoeia. Results:The impurity profile of clozapine from domestic and abroad was basically the same, and that of clozapine and its preparations was also basically the same. The method in United States pharmacopoeia was better than that in Chinese pharmacopoeia in terms of in terms of separation of the impurities. Conclusion: The current legal inspection standard for the related substances in clozapine described in Chinese pharmacopoeia should be improved.
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Objective: A new HPLC gradient elution was studied for the determination of notoginsenoside R 1, ginsenoside Rg 1 and Rb 1 in Xuesaitong Dripping Pills. Methods:C 18 column was used with a mobile phase of acetonitrile water 0～15 min. of (20∶80～40∶60) gradient elution, post time was 5 min, the wavelength of detecter was set at 203nm. Results: The linear range of R 1, Rg 1 and Rb 1 was 1.02～9.18?g,4.8～ 43.4?g and 4.6～41.6?g, respectively, the average recovery rate was 101.0% ( RSD =3.18%), 99.5%( RSD =3.02%) and 100.0%( RSD =1.19), respectively. Conclusion: The method is rapid, accurate, sensitive and relieble. The results show that the method can be used to control quality of products.