液相色谱在蝴蝶花植物药和甲基红霉素合成药分析中的

1O657.72UDC543.72StudyontheApplicationofHPLCinAnalyzingIrisJaponicaThunbandClarithromycinAThesistotheSchooloflifescienceandtechnology,BeijingInstituteofTechnologyFortheMasterDegreeofEngineeringByZhangJinzhuanSupervisedbyProfessorLuoAi’qinBeijingInstituteofTechnology,Beijing,China3HPLCHPLCHPLCHPLCpHHPLCHPLCHPLC1427HPLC4HPLCRPHPLCUSP:,,,4AbstractThethesismainlyfocusontheanalysisoftrad.Ch.MedicineIrisJaponicaThunbandsyntheticdrugclarithromycin.Fivesectionsareincluded.1.ThedevelopmentofHPLCsystemanditsuseinanalyzingoftrad.Ch.Medicineandsyntheticdrugswerereviewedandtheanalyticalworkdonebyformerresearcherswasalsosummarized.2.AHPLCmethodtoanalyzingIrisJaponicaThunbwasestablishedbyadjustingthetypeoforganicphase,theratiooforganicphaseandaquaticphase,pHvalue,flowrate,thetypeofbufferofthemobilephaseandthedetectivewavelength.3.TheHPLC-FPS(FingerPrintSpectrum)ofIrisJaponicaThunbwasestablishedbyanalyzingoffoursamplesextractedfromtherootofIrisJaponicaThunbbydifferentpersonindifferenttime.4.14samplesofIrisJaponicaThunbrootsand27samplesofIrisJaponicaThunbleaveswereanalyzedandtheactivecomponentforlowingbloodglucoselevelwasfounded.5.ARP-HPLCmethodwasdevelopedtoanalyzethecontentofclarithromycinandthestabilityofthemethodwasevaluated.Tenbatchesofsyntheticclarithromycinanditsrelatedsubstancewereanalyzedusingthismethod.Twoimpuritieswerefoundedinthesyntheticclatithromycin.Keyword:HPLC,IrisJaponicaThunb,HPLC-FPT,Clarithromycin51.11.2HPLC1.3HPLC1.3.1HPLC1.3.3HPLC1.4HPLC1.4.1HPLCHPLC1.51.622.3.12.3.22.3.362.3.42.433.13.23.2.13.2.23.2.33.34.14.24.2.14.2.24.2.374.2.44.34.44.4.14.4.24.4.34.4.44.4.4.14.4.4.24.555.15.385.45.55.65.791011121314151685ABC868788899012919293949596979899100171011025103104105106B1B2107108109110111112113114102115181920212223242526272829303132332.12.23435)36)-100%19372383940pH1.0mL/min411.5mL/min1.0mL/min1.5mL/min1.0mL/min2.222.23300nm424344PurityAnglePurityThresholdPurityAngle090PurityThreshold090PurityAnglePurityThresholdPurityAnglePurityThreshold2080VVpH2.871.0mL/min300nm2.1PurityAnglePurityThresholdPurityAnglePurityThreshold45pHAlltechC184.6mm250mm,5Alltech2080VVpH2.871.0mL/min300nm46[1]L.R.J.L.J.J.19982.20003.200247HPLC11923Waters515717996HPLC515717996Milliennium32WatersBranson2200BransonicUltrasonicsHempingFA1004PHS3BpHMFGCORPU.S.AJ.TBakerHPLC(AR)ARARAR308085mg5mL0.45485mL200L1mLAlltechC184.6mm250mm,5Alltech2080VVpH2.871.0mL/min300nmHPLCRA()RARARA5%RARARARA0.3010.1250.3060.1040.2961.0470.2923.370————0.3100.946——0.3400.4680.3450.2750.3471.3050.3352.933490.3920.1250.3720.0250.3800.447——0.4441.2240.4491.1380.4160.7460.4472.973————0.4521.817——0.4850.2640.4890.1020.4940.2680.4890.3600.5161.0500.5171.0000.5232.8240.5182.5570.5421.8150.5431.7380.5482.1860.5451.9970.6180.4350.6170.3750.6210.6470.6190.5600.6410.5790.6420.5630.6480.4240.6420.490————0.6650.4510.6600.3430.7090.1110.7060.1270.7050.4200.7050.1070.7990.0500.8000.0830.8050.2750.8000.153——0.8360.1370.8390.2540.8330.1130.9460.1470.9430.1580.9460.2410.9430.1471.0001.0001.0001.0001.0001.0001.0001.0001.1720.1711.1640.173——1.1630.120——1.5950.098——1.5150.1631.8553.7161.8353.7151.8089.6951.8357.070——1.9890.1541.9540.2341.9860.1202.1071.8172.0961.7922.0772.0882.0932.163——2.4370.1792.3740.2612.4320.3402.7401.3172.7141.5232.6711.6202.7091.6232.8053.9802.7923.7522.7584.0712.7844.510182222225%5081.8%-90.9%/%9010090.981.8RA5891720222425RA%123456780.4440.5160.5421.0001.8552.1072.7402.8051.2241.0501.8151.0003.7161.8171.3173.98080.230.4490.5170.5431.0001.8352.0962.7142.7921.1381.0001.7381.0003.7151.7921.5233.75281.420.4160.5230.5481.0001.8082.0772.6712.7580.7462.8242.1861.0009.6952.0881.6204.07171.480.4470.5180.5451.0001.8352.0932.7092.7842.9732.5571.9971.0007.0702.1631.6234.51071.68NRA51Mean+SD70%ErrorBarsshowMean+/-1.0SDBarsshowMeans12345678Peak2.0004.0006.0008.0001.5201.8581.9341.0006.0491.9651.5214.078ErrorBarsshowMean+/-1.0SDBarsshowMeans12345678Peak0.5001.0001.5002.0002.5000.4390.5190.5451.0001.8332.0932.7092.785522.70.2950.2950.4390.5190.5421.0001.8332.0932.7092.785No.No.1No.2No.3No.4No.5*No.6No.7No.8No.90.295**0.439**0.519**0.542**1.000**1.833**2.093**2.709**2.785***No.5**100%531..1988,136392.19.1988,23118393.HPLCFPS.1997,1130.54Waters515717996HPLC515717996Milliennium32WatersBranson2200BransonicUltrasonicsHempingFA1004PHS3BPH(MFGCORPU.S.AJ.TBakerHPLC(AR)ARARAR555614.395%60%ACE5780%95%95%95%IIIII95%OPI50%100%XYZ58L16(423)5.0g1611641%80,20%20%1%8068152050ml70ml0.45AFHMCDEIJKLAEF4.1ACDEFHI/mg18.818.524.561.127.117.416.5JAEFKLM/mg17.26.234.344.755.008.754.75IIIIIOPIEIIOXNIACIIIP150.454.2160.454.359ACEIIIIIOPXYZNI/mg30.711.812.618.115.83.17.510.511.612.010.515.612345678/mg5.25.55.46.74.67.88.65.9910111213141516/mg12.313.010.26.49.27.22.57.2AlltechC184.6mm250mm,5Alltech2080VVpH2.871.0mL/min300nmHPLC6061624.3.1.3.12-4.14634.3.1.4.15-4.1764651123456789A2.7033.5224.0694.2627.78714.07716.17020.79921.478C4.11214.42116.56621.20821.911D3.5944.13114.57216.70321.59822.248E2.6803.60915.25517.29623.057F2.7033.6104.2084.43315.28517.30523.014H2.2733.6244.435I2.7183.6694.2714.456J2.6903.