| Objective: To complete the quality standard of Ejiao Qianggu Oral Solution,establish its perfect quantitative identification methodology and the method of Oral liquid clarity of process optimization,and provide the basis for oral liquid internal quality control and evaluation.Methods: 1.Qualitative method as follows,to establish an analytical method for identification of donkey-hide gelatin in Ejiao Qianggu Oral Solution.Identification of donkey-hide gelatin in Ejiao Qianggu Oral Solution was established by HPLC-MS to triple quadruple mass spectrometry(QQQ-MS)methodologically inspected.2.Quantitative method as follows:(1)To establish a method of pre-column derivatization HPLC for testing components like L-hydroxy proline,glycine,alanine,L-prolinee simultaneously in Ejiao Qianggu Oral Solution and methodologically inspected.(2)To establish a wet digestion-atomic absorption spectroscopy method for determination of heavy metals plumbum,cadmium,hydrargyrum,arsenic and cuprum in Ejiao Qianggu Oral Solution from different batches so as to determine the residue of heavy metals and methodologically inspected.(3)To verify the ELSD-HPLC method for testing astragaloside IV in Ejiao Qianggu Oral Solution.3.Oral solution clarity of process optimization as follows,to change the clarity of oral liquid through the impact of chitosan on clarity.Results:(1)The HPLC-MS identification is gelatin mass spectrometry and chromatographic conditions as follows,Chromatographic separation was carried out on an ACQUITY UPLC BEH-C18 reversed phase analytical column(100mm×2.1mm,1.8 ?m particle size)at a column temperature of 40?.The injected sample volume was 5 ?L.The mobile phase consisted of 0.1% formic acid in water(eluent A)and acetonitrile(eluent B)in gradient elution.A flow rate of 0.3 mLˇmin-1 was employed for elution.Collagen marker peptides were detected by mass spectrometry in the positive electrospray ionization with multiple reaction monitoring(MRM).(2)Using high performance liquid chromatography method for determining the content of four kinds of amino acids in preparations,chromatographic conditions were as follows,Samples were hydrolyzed with hydrochloric acid at 105? for 24 h,and analysis was conducted by use PITC as reagent.Using Waters Welch XB-C18 column(4.6 mm×250 mm,5?m)with a gradient solvent system of the mobile phase A(0.1 molˇL-1 Sodium acetate buffer(pH6.5)solution acetonirirle;(93:7),the mobile phase B(solution acetonirirle: water;4:1).The flow rate was 1 mLˇmin-1.The detecting wave length was 254 nm.The injection volume was 5 uL and the drift tube temperature was 43?.(3)Using "Chinese pharmacopoeia" 2010 version of the general principles of the quantitative method(AAS)of heavy metals on the determination of lead,cadmium,mercury,arsenic,copper,can be used as a strong gelatin bone quantitative methods of heavy metal residues in the oral liquid.(4)The ELSD-HPLC for astragalus glycosides content method accurately,a good specificity.(5)Determined by experiments,the best flocculation process as follows,the mixture of chitosan acetic acid: water: a solution of chitosan=1:100:1,in the extract according to the proportion of 1.0 mL /100 m L to join the chitosan solution,stirring evenly,after 20? water bath stand for 16 h,under the speed of 6000 r?min-1 centrifugal 12 min,with two layers of filter paper suction filter after five times,made into oral liquid,transparent degree is relatively good.Conclusion: Through the above qualitative and quantitative clarity of process optimization for oral liquid quality standard is reasonable and feasible,can be used as quality control index of preparation. |
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