| Tanchuanbanxia granules are made of by 24 kinds of herbs such as Rhizoma pinelliae preparatum,Radix paeoniae alba,Lignum aquilariae resinatum,Radix angelicae dahuricae,Fructus schisandrae chinensis,Semen ziziphi spinosae,Radix glycyrrhizae,Herba asari,Cinnabaris,grind the Cinnabar into powder by water,grind 10 kinds of herbs such as Rhizoma pinelliae preparatum,Bulbus fritillariae cirrhosae,Cortex cinnamomi,and so on into fine powder,boil 12 kinds of herbs such as Radix glycyrrhizae,Radix angelicae dahuricae,Fructus schisandrae chinensis,and so on twice,filtrate concentrated into a paste,add above-mentioned powder,mix well,granulating,drying,sieving,spray menthol oil.It has the function of relieving cough,dissipating phlegm and relieving asthma.Used in the treatment of new and old cough,phlegm and asthma.3 g per bag.Because the current quality standard control project of this variety is too simple,and the products produced by the enterprise have no effective quality control methods,resulting in large quality differences among different batches,it is necessary to improve the quality standard.The improvement of quality standard of Tanchuanbanxia granules was studied in this paper.The quality standards were established from six aspects:prescription and preparation method,microscopic identification,TLC identification,Liquid chromatograph identification,examination,content determination and fingerprint.The prescription and preparation method followed the original standard medicine flavor and process.In order to facilitate production,the total amount of 1800 g in the original prescription was unified to 1000 g,and the amount of each medicine flavor in the prescription was converted.Cinnabar 13.3g was ground by water flies into a very fine powder for reserve;crush Rhizoma pinelliae preparatum 266.7g,Bulbus fritillariae cirrhosae 26.7g.Cortex cinnamomi 26.7g,Fructus amomi rotundus(shelled)26.7g,Lignum aquilariae resinatum 26.7g,Flos caryophylli 26.7g,Radix panacis quinquefoll 26.7g,Radix angelicae dahuricae 106.7g,Herba asari 106.7g,Bambusae concretio silicea 10 g into fine powder,mix with the Cinnabar powder.Pericarpium citri reticulatae 160 g,Rhizoma chuanxiong 106.7 g,bran fried Fructus Aurantii 106.7 g,bran stir-fry Rhizoma atractylodis macrocephalae 106.7 g,bran fried Pericarpium citri reticulatae viride 106.7 g,Rhizoma alismayis 106.7 g,bran fried Radix paeoniae alba 106.7 g,Fructus crataegi 106.7 g,made Fructus schisandrae chinensis 106.7 g,Semen ziziphi spinosae 106.7 g,Rhizoma zingiberis 71.1 g,decoction twice with water.the first 4 hours,the second 3 hours,combined decoction,filtration,filtrate concentrated into clear cream,mix well,granulating,drying,sieving,spray add menthol oil,made of 1000 g.The total amount made in the original prescription was 1800 g,which was uniformly 1000 g for production convenience.Rhizoma pinelliae preparatum,Bulbus fritillariae cirrhosae,Cortex cinnamomi,Fructus amomi rotundus,Lignum aquilariae resinatum,Cinnabaris were identified by microscopical identification.The six kinds of higher visibility parts such as large calcium oxalate needle bundle(pinellia ternata),starch granule(fritillary bulb)and stone cell(cinnamon),Endosperm cell starch mass(cinnamomum),bordered pit vessel(agarwood),Cinnabaris are included in the draft standard.Thin layer chromatography(TLC)was used to qualitatively identify the raw materials of the Radix paeoniae alba,Radix angelicae dahuricae,Fructus schisandrae chinensis and Semen ziziphi spinosae,the control materials and control materials were used for random control.Results the repeatability and reproducibility of Radix paeoniae alba,Radix angelicae dahuricae,Fructus schisandrae chinensis and Semen ziziphi spinosae were better,10 batches of samples can be detected,so the four kinds of TLC identification are included in the draft standard;A high performance liquid chromatography(HPLC)method was used to identify the Aloes tetraol of Lignum aquilariae resinatum,at the same time,the characteristic peaks in the control medicine of Lignum aquilariae resinatum were compared simultaneously and separated by C18 column,Acetonitrile-0.5%phosphoric acid aqueous solution was used as mobile phase,gradient elution and detection wavelength of 250 nm.The results showed that 10 batches of samples showed characteristic peaks of agilawood tetra-alcohol and agilawood.Therefore,HPLC method was included in the dra ft standard for the identification of agilawood.Aristolochic acid A in tanchuan banxia granules was determined by HPLC.Octadecyl silane bonded silica gel was used as the filler,and the chromatographic column was eluted by acetonitrile-0.5%phosphoric acid solution(38:62)with a detection wavelength of 320 nm.The number of theoretical plates calculated according to the aristolochic acid A peak should not be less than 5000.Results:the specificity test was negative and no interference was detected in 10 batches of samples.Considering the necessity to control the toxic components,the content limit was included in the draft standard.The content limit was set according to the daily dose,and the content of aristolochic acid A(C17H11NO7)in each bag should not exceed 1.00μg.Pb,Cd,As,Hg,Cu in tanchuanbanxia granules were determined by ICP-MS.Following the general rule 2321 of 2015 pharmacopoeia,Pb 0.03 μg/g,Cd 0.02 μg/g in 10 batches;As not detected;Hg 8398.39μg/g;Cu 5.03 μg/g.The contents of Pb,Cd,As and Cu are far below the standard,so these four elements are not included in the standard text.Hg basically comes from cinnabar which is not only the active component but also the toxic component.Therefore,it is included in the draft standard and set the upper and lower limit.Each bag should contain 20.2～33.8 mg of Hg.HPLC method was used to determine the content of paeoniflorin,agalloch eaglewood,glycyrrhizin,glycyrrhizic acid and schisandrin a in Tanchuanbanxia granules.Chromatographic column with octadecyl silane bonded silica gel as filler;Acetonitrile was used as mobile phase A,and 0.1%formic acid solution was used as mobile phase B.Gradient elution(0 min,15%A;24 min,18%A;28 min,38%A;59 min,47%A),detection wavelength:218 nm(schisandrin A),235 nm(paeoniflorin),250 nm(agarwood tetranol,glycyrrhizin),272 nm(glycyrrhizin),the number of theoretical plates calculated according to the peak of paeoniflorin should not be less than 15,000.Results:the specificity test was negative without interference.Paeoniflorin,aloes four alcohol,liquorice glycosides,glycyrrhizic acid,fructus schisandrae alcohol armour in the range of 194.6～6811.0 ng,41.06～1437.1 ng,97.08～3397,8 ng,80.7～2824.5 ng,3.33～116.55 ng,the linear relationship is good,10 batches of samples paeoniflorin and aloes four alcohol,liquorice glycosides,glycyrrhizic acid,the average content of fructus schisandrae alcohol armour per bag respectively 5.36,1.27,2.59,2.22,0.11 mg.Schisandra chinensis has a low content of schisandra chinensis and its peak area is too small to be included in the draft standard,while the other four components are included in the draft standard.The content lower limit is set as:each bag containing salvia miltiorrhiza sodium(C9H9NaO5)shall not be less than 4.3 mg.Each bag shall contain agarwood in the form of agarwood tetrahydrol(C17H18O6),not less than 1.0mg;Glycyrrhizic acid(C42H62O16),not less than 1.8 mg,and glycyrrhizin(C21H22O9),not less than 2.0 mg per bag.HPLC method was used to establish the fingerprint of Tanchuanbanxia granules.Standard fingerprint was generated from 10 batches of samples and the homogeneity of all samples was evaluated at one time.The chromatographic column was filled with octadecyl silane bonded silica gel,acetonitrile as mobile phase A,0.1%phosphoric acid solution as mobile phase B,and gradient elution(0 min,7%A;20 min,17%A;35 min,24%A;45 min,41%A;70 min,58%A);The detection wavelength was 235nm,and the similarity of 10 batches of Tanchuanbanxia granules was analyzed,and the result was between 0.886～0.995.In addition,high performance liquid chromatography-time of flight mass spectrometry(LCMS-Q-TOF)was used to qualitatively analyze the chromatographic peaks in the fingerprint of Tanchuanbanxia granules.The ion source of mass spectra was electrospray ion source(ESI),and the multi-level mass spectra data of each component were obtained by using positive and negative ion detection modes respectively.Using mass spectrometry cracking law and literature data,determine the identity of the 17 chromatographic peak,1(gallic acid),5(tanshinol),9(S)(paeonia lactiflora lactone glycosides),10(paeoniflorin),11(licorice glycosides),12(gallic acid paeoniflorin/gallic acyl peony lactone glycosides or its isomer),13(rosemary acid),14(purple oxalic acid decarboxylation products),15(Dan phenolic acids B). |
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