The Study of Analytical Method about Multicomponent Preparation

Abstract: The Compound Reserpine Tablets can cure hypertension,it is one multicomponent preparation.Its effective components are Reserpine、Hydrochlorothiazide and Dihydralazine sulfate.There are only the identication test for the effective components in National Medical Criterion WS-10001-(HD-1352) -2003 of State Food and Drug Administration,To establish two method for analyzing Compound Reserpine Tablets for to control its quality.The first method was HPLC,the second method was Partial least square(PLS).HPLC was established for the determination of three compounds in compound reserpine tablets.The determination of Reserpine、Hydrochlorothiazide was performed on Shim-Pack CLC-CN column(5um,4.6mm×250mm),the mobile phase of determining Reserpine and Hydrochlorothiazide consisted of 0.01mol/L sodium heptanesulfonate solution—acetonitrile(6:4)(adjust pH to 2.7 with phosphoric acid);Dihydralazine sulfate was performed on Shim-pack VP-ODS (5um,4.6mm×150mm),the mobile phase of Dihydralazine sulfate consisted of 0.06%sodium hexanesulfonate and 0.04%sodiumheptane sulfonate-acetonitrile -methanol(65:15:20)(adjust pH to 3.0 with phosphoric acid);The UV detection wavelength of Reserpine、Hydrochlorothiazide and Dihydralazine sulfate was set at 220nm、265nm、310nm respectively;Thesample size was 50μl、10μl、20μl respectively;The flow rate was 1.0ml/min.The linear range about the content of Reserpine、Hydrochlorothiazide and Dihydralazine sulfate was 2.5μg/ml~3.99μg/ml(r=1.0000)、24μg/ml~37μg/ml(r=1.0000)、33μg/ml~50μg/ml(r=1.0000) respectively;The average recovery was 100.7%、100.0%、99.01%respectively; RSD was 0.06%、0.04%、0.10%(n=6) respectively.The linear range about the dissolution of Reserpine、Hydrochlorothiazide and Dihydralazine sulfate was 0.22μg/ml-0.41μg/mL(r=1.0000)、21μg/ml-39μg/ml(r=0.9999)、29μg/ml-55μg/ml (r=1.0000) respectively;The average recovery was 100.1%、99.47%、99.49%, respectively;RSD was 0.06%、0.04%、0.10%(n=6) respectively.The method could be used to determine the uniformity.A partial least squares(PLS) method was established for the determination of six compounds in Compound Reserpine Tablets.The UV detection wavelength was 240~340nm.The average recovery of reserpine hydrochlorothiazide,dihydralazine sulfate,vitamin B_1,vitamin B_6 and promethazine hydrochloride was 101.1%, 100.4%,99.69%,100.4%,98.99%,99.36%,respectively,with the RSD of 0.65%, 0.63%,1.03%,0.81%,0.49%and 0.83%respectively.The linearity of Six components was good in 70%~130%of content.The method could be used to determine the uniformity and the dissolution.The two method has not prominent difference by comparing the result of the two method.The conclusion:HPLC could avoid disturbing of coexistence component,and Partial least square could be used to analyze spectra overlapping multicomponent without any pre-separation.Establishment of the two analytical method could perfect the Medical Criterion for Compound Reserpine Tablets,this would help to provide reference for revising the Medical Criterion…
Key words: high performance liquid chromatography(HPLC); Partial least square(PLS); Compound Reserpine Tablets; Reserpine; Dihydralazine sulfate; Hydrochlorothiazide

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