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(~):(~):(~)Tablele151 Result of precision experiment(Time,Rtime)Peakno.Time/Rtime(min)RSD(%)1234512340506789101112Table152 Result of precision experiment(Area,Rarea)Peak no.Area/RareaRSD(%)123451135402223853212535203806198102259251655876505783002642213358114167445601110735287694326369/328621/337879/338415/324127/5352541/385341/366265/377012/379119/61394426/1414983/1413478/1376039/1466960/71539480/11574380/11538928/11549105/11579661/18654279/652634/675358/688065/686874/9925436/950210/966810/953504/960168/1021014013926722330013636614407911458217/456661/472371/452541/483297/122760129191297162687027104Table161 Result of stability experiment(Time,Rtime)Peakno.Time/Rtime (min)RSD( %)0h3h6h9h12h123456789101112 Tablele162 Result of stability experiment(Area,Rarea)Peak no.Area/RareaRSD(%)0h3h6h9h12h1234567891011121354025925135811338685/344843/1394426/1539480/1689687/925436/210140458217/2760120380683002110735338415/356294/1376039/1549105/1697097/953504/136366452541/26870908455085752168342294/362907/1419388/1592066/1743801/1006564/149474462662/24301782384805650241338245/376692/1447205/1585939/1731793/989950/143847486379/28367765545271854016336744/362977/1453593/1603544/1742497/997517/136924487693/30836Table171 Result of preproducibility experiment(Time,Rime)Peak no.Time/Rtime(min)RSD(%)12345123456789101112 Table172 Result of preproducibility experiment(Area,Rarea)Peak no.Area/RareaRSD(%)123451255900146966278478283106191604210404677423114718112559890253688565104681425276560523924379208/352018/389051/365225/362645/5414286/378454/425077/373867/389162/61676873/1558681/1772186/1560033/1549120/71793447/11700105/11889234/11698725/11665721/18773075/766747/874715/776317/757903/91150254/1081267/1241558/1112190/1113204/1018384712886518298415979815709911466296/424776/486833/453560/441416/126960340703622475853061730Table 181 Fingerprint result of ten tablets halfproduction(Time/Rtime)PeakNO.Sample Time/Rtime(min) 1 2 3 4 5123456789101112678910xmin ? xmax ? ? 1Table 182 Fingerprint result of ten tablets halfproduction (Area/R?area)PeakNO.Sample Area/R?area1234512345678910111225589610404668853379208/414286/1676873/1793447/1773075/1150254/183842466296/6965920265512482494043375002/354222/1685851/1816391/1633012/1181432/194641585032/725602339018776457719318976/287251/1445156/1506833/1606610/884091/96304360118/469491469647742351044352018/378454/1558681/1700105/1766747/1081267/12866424776/4070127847611471581420389051/425077/1772186/1889234/1874715/1241558/182981486833/62249678910xmin ? xmax28311011255881423365225/373867/1560033/1698725/1776317/1112190/182984453560/622471916018902452391362645/389162/1549120/1665721/1757903/1113204/157098441416/617331941529367563183340821/355630/1554113/1798020/1630220/1149482/105144521156/5079423189710577686282405772/431367/1781327/2076921/1776344/1337970/143550575181/730864454511851072589284020/249069/1613517/1766998/1811043/986257/248348461324/32205???1???第二節(jié) 指紋圖譜相似度計算1. 相似度計算原理及公式 相似度可以量化描述指紋圖譜相似性,即客觀的數(shù)字化描述?! ? ?。短柟┰囈?,連續(xù)進樣5次,按 ,檢測指紋圖譜。C提前1min,見附圖2)。l進樣,分別以甲醇-水,乙腈-水,甲醇-水-磷酸,乙腈-水-磷酸不同梯度進行試驗,記錄色譜圖,結(jié)果表明乙腈-水以表14梯度進行試驗,色譜圖分離效果最佳。8. 樣品中對照品的含量測定 分別精密稱取10批樣品,甲醇溶解并定容至100ml,測定峰面積,利用標準曲線法計算洋金花有效部位中對照品的含量。 Table9 Result of precision experiment of the method (n=5) NO. 1 2 3 4 5 area 522555 515547 517423 509990 510808 area 515265 RSD% 由表9可知,測定結(jié)果的RSD%=%,表明儀器系統(tǒng)的精密度高。l, 11181。C;流速:1ml/min;理論塔板數(shù):不低于4000。Table 6 Result of recovery experiment of the method (n=5)NO. a(mg) b (mg) c(mg) d (%) e(%) 1 2 3 4 5 a 已知樣品中總黃酮的含量 b 對照品的加入量 c 加入對照品后樣品中總黃酮的測得量 d 加樣回收率 e 平均加樣回收率 由表6可知,%,表明該方法可行。Fig3 normal curve of standard material5. 精密度實驗 精密稱取對照品1mg,甲醇溶解并定容至50ml,連續(xù)重復測定5次時,測定結(jié)果見Table3。–NMR中的化學位移,推斷其苷鍵為α構(gòu)型。其1H–