ABSTRACT
HPLC-RID and HPIC-CD methods were established for the determination of sucrose octasulfate content in irinotecan hydrochloride liposomes for injection. HPLC-RID: This method was performed on a Kromasil 100-5-NH2 column (250 mm×4.6 mm, 5 μm) with a mobile phase of 0.8 mol·L-1 ammonium sulfate buffer (pH 3.5)-acetonitrile (83∶17). The flow rate, column temperature and detector temperature were maintained at 1 mL·min-1, 30 ℃ and 30 ℃ respectively. HPIC-CD: This method was performed on an anion exchange column Dionex InPacTM AS11-HC (250 mm×4 mm, 9 μm) with an eluent of 30 mmol·L-1 sodium hydroxide solution. The flow rate was 1.5 mL·min-1, the column temperature was 30 ℃ and the detector temperature was 35 ℃. The HPLC-RID method and HPIC-CD method were validated with respects to specificity, limit of detection, limit of quantitation, linearity, precision, accuracy, stability and robustness and met the validation requirements. There were no significant differences between the HPIC-CD and HPLC-RID methods according to T-test analysis, both of which were applicable for the measurement of sucrose octasulfate concentration in irinotecan hydrochloride liposomes for injection. However, the HPLC-CD was better at the following aspects: higher detection sensitivity, simpler sample pretreatment, lower time and money spent, better environmental protection.
ABSTRACT
Objective: To study the relative molecular mass and composition of Ligustrum lucidum polysaccharide purified by dialysis, and provide the theories for the relationship between the biological activity and the internal composition. Methods: In this paper, L. lucidum as an object was studied. Polysaccharide was isolated by water extraction and ethyl alcohol precipitation and purified by Sevage method, hydrogen peroxide and dialysis. After the acidolysis of trifluoroacetic acid, the molecular weight was measured by GPC, and the composition of polysaccharide was analyzed by HPLC-RID. Results: The Mw of polysaccharide was 10 721, and the Mn of polysaccharide was 10 673. L. lucidum polysaccharide consisted of glucose, rhamnose, and arabinose, the molar ratio of these monosaccharide was 9.148.105.18. Conclusion: The purified polysaccharide composition is more homogeneous, and the monosaccharides of polysaccharides was easily analyzed by HPLC-RID without column derivatization.
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Objective:To establish an HPLC-RID method for the simultaneous determination of taurine and aminocaproic acid in compound taurine eye drops. Methods:A Waters NH2column(250 mm ×4.6 mm,5 μm) was used, the mobile phase was water-acetonitrile (40:60) at a flow rate of 0.8 ml·min-1, the column temperature was 35.0℃, and the temperatures of the detector reference cell and the sample cell were both set at 35.0℃,The injection volume was 20 μl. Results:The linear ranges of taurine and aminocaproic acid were 0.05-2.00 mg·ml-1(r = 0.999 9). The average recovery was 98.57% (RSD = 1.07%,n= 9) and 100.69% (RSD =0.75%,n =9),respectively. Conclusion:The established method is accurate,simple and rapid, and suitable for the quality control of compound taurine eye drops.
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Objective To establish a method for determination of accessories lactose by HPLC-RID.Methods Boston Green Amino-NH2 column (250 mm× 4.6 mm,5 μm) was used.The mobile phase was acetonitrile-water (70:30).The flow rate was 1.0 mL/min.The column temperature was 45 ℃,the detector temperature was 40 ℃ and the injection volume was 10 μL.Results Lactose showed good linearity in the range of 0.2-5.0 mg/mL (r≥0.999 8).The detection limit was 0.06 mg/mL.The average recovery was 99.6％ and the relative standard deviation was 0.7％.Conlusion The method is specific,convenient,fast and accurate,which can be used for determination of accessories lactose.
ABSTRACT
Objective To establish a method for determination of accessories lactose by HPLC-RID.Methods Boston Green Amino-NH2 column (250 mm× 4.6 mm,5 μm) was used.The mobile phase was acetonitrile-water (70:30).The flow rate was 1.0 mL/min.The column temperature was 45 ℃,the detector temperature was 40 ℃ and the injection volume was 10 μL.Results Lactose showed good linearity in the range of 0.2-5.0 mg/mL (r≥0.999 8).The detection limit was 0.06 mg/mL.The average recovery was 99.6％ and the relative standard deviation was 0.7％.Conlusion The method is specific,convenient,fast and accurate,which can be used for determination of accessories lactose.
ABSTRACT
OBJECTIVE:To establish a method for determination of dextran70 in Compound dextran70 eye drop. METHODS:HPLC-RID was performed on the column of Phenomenex PolySep-GFC-P 4000 with the mobile phase of 0.7% Na2SO4 solution. The flow rate was 0.5 ml/min,column temperature was 35 ℃ and injection volume was 50 μl,and the inner temperature of refrac-tive index detector was 40 ℃. RESULTS:The linear range of dextran70 was 0.1-5.0 mg/ml(r=0.999 5);RSDs of precision,sta-bility and reproducibility tests were lower than 2%;average recovery was 97.45%-101.76%(RSD=0.57%,n=9). CONCLU-SIONS:The method is simple,fast and reliable with high separation and short analysis time,and can be used for the content deter-mination of dextran70 in Compound dextran70 eye drop.