Диссертация (Изучение травы Inula Viscosa (L.) с целью создания экстракта и геля для местного и наружного применения), страница 25

Пик с временемудерживания 14.02 мин имеет молекулярный вес 332 и предположительноимеет структуру Quercetagetin 3'-methyl ether:160N3N4MR-RUDN-250717-5 16785 (13.989) Cm (16732:16832-16861:16882)2: Diode Array2.487e-2372.8256.8MR-RUDN-270717-1 16855 (14.047) Cm (16806:16914-16741:16768)Quercetagetin 3'-methyl ether2.25e-22.0e-2222.8O220.81.6e-2CH31.4e-21.75e-2OH1.2e-21.5e-2369.8HO1.25e-2AUAU2: Diode Array1.895e-2256.81.8e-2O1.0e-28.0e-31.0e-27.5e-3HO5.0e-36.0e-3OH4.0e-3OHO8009002.0e-32.5e-30.0100200300400500600700MR-RUDN-250717-6 1651 (14.000) Cm (1646:1657-1640:1644)1000110012001300331.1100m/z14001: Scan ES1.10e60.0100200300400500600700MR-RUDN-270717-2 1659 (14.069) Cm (1655:1666-1648:1651)8009001000110012001300263.1100m/z14001: Scan ES8.66e5331.0263.5331.4%%331.2331.7332.0332.0332.5262.8264.0333.5168.3 169.3206.7168.7332.2263.1168.7198.8333.0 399.5483.2815.6 858.0602.5 663.70100200300400500600700MR-RUDN-250717-5 1658 (14.058) Cm (1650:1660-1642:1647)800972.69001017.010001065.81220.6110012001300333.7100m/z14001: Scan ES+1.01e7583.2583.4628.9457.3551.21026.7732.5 836.7 858.9 927.4 954.00100200300400500600700MR-RUDN-270717-1 1662 (14.093) Cm (1655:1669-1649:1652)1292.91000110012001000110012001349.01419.11300m/z14001: Scan ES+4.28e6334.0334.1247.7%900333.6100%800333.3142.6 247.5334.4201.8334.5266.0334.5334.9335.3142.5335.8229.7 247.6335.7 437.80100m/z200300400592.0 614.0 657.4920.6354.3010050060070080090010001100120013001400781.11220.7900.6m/z20030040050060070080090013001400Пик с временем удерживания 14.16 мин имеет молекулярный вес 316 ипредположительно имеет структуру 3-Methylquercetin (в соответствии слитературными данными):N3N4MR-RUDN-250717-5 16950 (14.126) Cm (16903:16996-17090:17139)219.82: Diode Array MR-RUDN-270717-1 17018 (14.183) Cm (16968:17068-17116:17196)346.83.453e-2344.8isorhamnetin3.0e-22.0e-2O2.5e-2252.8CH32: Diode Array2.22e-2219.81.75e-21.5e-2OH2.0e-2253.8HOAUAU1.25e-2O1.0e-21.5e-27.5e-3OH1.0e-25.0e-3OH5.0e-3O2.5e-30.0100200300400500600700MR-RUDN-250717-6 1668 (14.144) Cm (1660:1679-1684:1688)8009001000110012001300315.11000.0m/z14001002003004005006007008001: Scan ES- MR-RUDN-270717-2 1677 (14.222) Cm (1670:1685-(1689:1696+1660:1668))193.09.44e510090010001100120013001000110012001300110012001300m/z14001: Scan ES1.03e6315.1315.5%%315.5237.5315.8169.3265.1 315.9193.5316.4168.9435.0463.7331.2333.2264.8162.9591.2631.1857.6 907.80100200300400500600700MR-RUDN-250717-5 1670 (14.159) Cm (1663:1679-1686:1692)800900316.7 475.5 497.11326.61000110012001300317.7100238.0 316.5168.8575.7631.41317.4876.3m/z014001002003004005006007008001: Scan ES+ MR-RUDN-270717-1 1680 (14.246) Cm (1671:1683-(1639:1669+1685:1711))317.79.89e61009001410.5 1482.4m/z14001: Scan ES+1.01e7%%318.0318.5193.7318.6261.6318.3318.7193.5203.9319.3175.60100261.8327.9 388.6320.1 378.8m/z200300400500600700800900100011001200130014000100533.8975.3m/z20030040050060070080090010001400161Пик с временем удерживания 15.12 мин имеет такой же молекулярныйвес 316, но предположительно имеет структуру Nepetin, содержание которогоупоминается в литературных источниках:N3N4MR-RUDN-250717-5 18105 (15.089) Cm (18031:18190-17746:17963)2: Diode Array MR-RUDN-270717-1 18172 (15.145) Cm (18122:18225-17961:18017)255.86.667e-2255.8357.86.0e-2OH2: Diode Array7.546e-2356.87.0e-2219.8219.8O6.0e-25.0e-2OH3 C5.0e-24.0e-2OAUAUHO4.0e-23.0e-23.0e-2OH2.0e-2Nepetin2.0e-2OH1.0e-21.0e-20.0100200300400500600700800MR-RUDN-250717-6 1781 (15.103) Cm (1776:1788-(1749:1763+1796:1808))9001000110012001300315.01000.014001002003004005006007008001: Scan ES- MR-RUDN-270717-2 1787 (15.155) Cm (1783:1794-(1797:1806+1767:1777))315.13.01e6100m/z900100011001200130080090010001100120013008009001000110012001300m/z14001: Scan ES3.27e6315.5%%315.5316.0316.0267.1316.5267.1632.2383.1m/z9001000110012001300317.8631.3632.0383.0 415.4317.7100m/z14001: Scan ES+3.29e7%14001: Scan ES+3.09e70100200300400500600700MR-RUDN-270717-1 1790 (15.179) Cm (1785:1796-1755:1774)%100316.4169.1 265.1535.40100200300400500600700800MR-RUDN-250717-5 1782 (15.109) Cm (1778:1789-(1742:1767+1795:1818))318.6187.60100233.9291.7142.40100m/z20030040050060070080090010001100120013001400233.7291.9m/z2003004005006007001400Пик с временем удерживания 15.39 мин имеет молекулярный вес 346 иможет иметь структуру Tomentin (3,7-Dimethylquercetagetin):N3N4MR-RUDN-250717-5 18427 (15.357) Cm (18369:18498-18740:18890)219.84.5e-2OH2: Diode Array MR-RUDN-270717-1 18488 (15.408) Cm (18459:18519-18555:18583)219.84.552e-2OHO4.0e-2O351.86.0e-2CH3257.83.5e-22: Diode Array6.706e-2H3 C3.0e-2352.85.0e-2O257.8OOH2.0e-2AUAU4.0e-22.5e-23.0e-2OH1.5e-22.0e-21.0e-21.0e-25.0e-3Tomentin; 3,7-Dimethylquercetagetin0.0100200300400500600700800MR-RUDN-250717-6 1815 (15.391) Cm (1809:1820-(1821:1855+1765:1810))9001000110012001300344.91000.014001002003004005006007008001: Scan ES- MR-RUDN-270717-2 1819 (15.426) Cm (1816:1824-(1827:1845+1778:1815))345.01.85e6100m/z900100011001200130090010001100120013009001000110012001300m/z14001: Scan ES3.13e6345.5%%345.5346.0345.9346.1346.5168.9265.0265.6346.4266.3 330.5412.90100200300400500600700800MR-RUDN-250717-5 1814 (15.381) Cm (1809:1822-(1826:1839+1776:1810))9001000110012001300347.7490.4m/z14001: Scan ES+2.94e7%%100347.0m/z014001002003004005006007008001: Scan ES+ MR-RUDN-270717-1 1818 (15.416) Cm (1817:1828-(1794:1816+1833:1843))347.82.19e7100348.6348.7185.6 231.6369.7142.40100m/z200300400500600700800900100011001200130014000100249.8m/z2003004005006007008001400162Пик с временем удерживания 16.80 мин имеет молекулярный вес 300.Наосновании литературных данных извсех возможных изомеровпредпочтение можно отдать структуре Hispidulin:N3N4MR-RUDN-250717-5 20126 (16.773) Cm (20072:20199-19835:19995)2: Diode Array6.38e-2335.8219.86.0e-2MR-RUDN-270717-1 20194 (16.830) Cm (20148:20242-(20333:20391+19974:20067))2: Diode Array1.665e-1334.81.6e-1OH1.4e-15.0e-2HOO1.2e-1272.8H3 C219.81.0e-1OAUAU4.0e-23.0e-2OHO8.0e-26.0e-22.0e-2Hispidulin4.0e-21.0e-22.0e-20.0100200300400500600700800MR-RUDN-250717-6 1981 (16.799) Cm (1972:1988-(1992:2019+1941:1969))900100011001200299.01000.0100200300400500600700MR-RUDN-270717-2 1988 (16.859) Cm (1981:1994-1997:2018)m/z14001: Scan ES2.45e61300800900100011001200130080090010001100120013008009001000110012001300299.0100m/z14001: Scan ES4.80e6299.4%%299.4300.0300.1300.5283.9 301.0298.20100200300400500600700800MR-RUDN-250717-5 1982 (16.805) Cm (1976:1991-(1942:1967+1998:2020))m/z900100011001200130014001: Scan ES+1.95e7301.8301.8m/z14001: Scan ES+3.80e7%100%1000100200300400500600700MR-RUDN-270717-1 1998 (16.943) Cm (1982:1998-1945:1970)302.7289.7286.90100231.90100m/z20030040050060070080090010001100120013001400655.1m/z2003004005006007001400Пик с временем удерживания 20.66 мин имеет молекулярный вес 316 ипредположительно имеет структуру Rhamnetin:N3N4MR-RUDN-250717-5 24756 (20.633) Cm (24683:24836-(24288:24573+24977:25159))2: Diode Array1.723e-2369.8RhamnetinMR-RUDN-270717-1 24817 (20.683) Cm (24756:24883-(24941:25034+24639:24697))1.8e-2256.8OH1.4e-21.2e-2O1.2e-2AUAU367.81.4e-2O8.0e-3OH6.0e-3221.81.6e-2H3 C1.0e-22: Diode Array2.018e-2256.8OHOH1.0e-28.0e-3O6.0e-34.0e-34.0e-32.0e-32.0e-30.0100200300400500600700800MR-RUDN-250717-6 2438 (20.674) Cm (2428:2445-(2387:2420+2457:2492))9001000110012001300315.1100m/z14001: Scan ES7.56e50.0100200300400500600700800MR-RUDN-270717-2 2441 (20.700) Cm (2433:2449-(2454:2461+2424:2429))9001000110012001300110012001300315.1100m/z14001: Scan ES8.66e5315.5%%315.5299.2316.1316.0316.4299.0168.9169.3404.9459.7 495.4820.80100200300400500600700800MR-RUDN-250717-5 2448 (20.757) Cm (2432:2448-(2395:2422+2463:2492))1376.9940.6 1022.6 1116.19001000110012001300317.4460.0559.9193.0m/z317.8669.6724.9756.50100200300400500600700800MR-RUDN-270717-1 2450 (20.776) Cm (2437:2450-(2455:2466+2424:2436))908.3998.390010009001000317.8317.6 317.9100%14001: Scan ES+7.01e6%100316.5168.7169.5316.7m/z14001: Scan ES+6.12e6301.8318.4301.6318.4318.7142.6181.6196.3319.4158.50100301.3274.0273.6m/z200300400500600700800900100011001200130014000100319.3319.7391.7526.7 630.6 648.21070.41128.11268.31339.2m/z2003004005006007008001100120013001400163В фракции №3 присутствуют 4 пика с временами удерживания 8.21, 8.52,9.93 и 10.30 мин, которые отсутствуют в других фракциях и могут иметьструктуры Hyperoside, Quercetagetin 3'-methyl ether 3-glucoside, Isorhamnetin-3O-glucoside и Quercetagetin 3',4'-dimethyl-3-O-glucoside:N3MR-RUDN-250717-5 9850 (8.208) Cm (9824:9881-9617:9658)Hyperoside219.87.0e-2Quercetagetin 3'-methyl ether 3-glucosideN32: Diode Array8.197e-2255.88.0e-2MR-RUDN-250717-5 10228 (8.523) Cm (10187:10257-10287:10324)219.8256.81.4e-2351.86.0e-2OAUAU1.0e-2O4.0e-2OHOOH5.0e-23.0e-2HO1.2e-2OHO2: Diode Array1.671e-2OHOH353.8CH3OOHOHHO8.0e-3OOHOOOHO6.0e-3HO2.0e-2OH4.0e-3OH1.0e-22.0e-30.0100200300400500600MR-RUDN-250717-6 971 (8.234) Cm (969:974-935:946)700800900100011001200m/z14001: Scan ES5.71e61300463.0100OH0.0100200300400500600700800MR-RUDN-250717-6 1009 (8.556) Cm (1004:1012-(1015:1031+989:998))900OH1000110012001300493.1100m/z14001: Scan ES1.52e6463.5%%493.6494.1464.0494.3464.5927.4928.7462.2 465.0303.00100200300400500600MR-RUDN-250717-5 974 (8.258) Cm (968:976-940:952)700800900168.7100011001200m/z14001: Scan ES+1.04e71300303.6100495.0429.2491.3561.5 595.3267.3860.2 909.7 987.20100200300400500600700800MR-RUDN-250717-5 1010 (8.563) Cm (1005:1014-(1017:1033+987:1001))OH900O303.91041.0 1123.4100011001352.912001300333.71001489.3m/z14001: Scan ES+3.91e6CH3OHOH334.0HOO%%HOOH304.6OHO334.4HOOOH334.8OHO142.4305.3259.5142.60100306.4465.9487.7488.7142.6214.5 235.0417.5m/z200300400500600700800900100011001200130001001400Isorhamnetin-3-O-glucosideN3MR-RUDN-250717-5 11914 (9.929) Cm (11874:11951-11763:11832)219.8344.8O2.5e-22: Diode Array2.642e-2CH3908.41018.630040050060070080090010001100O354.814002: Diode Array2.14e-2CH3OCH3219.81.75e-2O1300Quercetagetin 3',4'-dimethyl-3-O-glucoside257.82.0e-2HO1.5e-21.5e-21348.21200MR-RUDN-250717-5 12354 (10.295) Cm (12299:12404-(12427:12515+12147:12229))2.0e-21378.51151.5m/z200N3OHHO517.9401.8335.8518.3453.7562.3 680.4780.4796.8OAU1.25e-21.0e-2OHAUOOOHOH2.5e-3OH9001000OHO5.0e-3OH110012001300477.1100O7.5e-35.0e-3OHOOHO0.0100200300400500600700800MR-RUDN-250717-6 1174 (9.955) Cm (1168:1180-(1186:1202+1153:1163))HO1.0e-2m/z14001: Scan ES3.00e6OH0.0100200300400500600700800MR-RUDN-250717-6 1215 (10.303) Cm (1208:1222-(1227:1233+1195:1204))OH90010009001000110012001300110012001300m/z14001: Scan ES1.75e6507.1100477.5%%507.6508.1478.1508.4478.6508.6506.4 508.9479.1577.2955.40100200300400500600700800MR-RUDN-250717-5 1176 (9.971) Cm (1170:1181-(1186:1200+1157:1165))461.19001000110012001300317.6100O14001: Scan ES+7.92e60100200300400500600700800MR-RUDN-250717-5 1218 (10.327) Cm (1210:1223-(1227:1237+1197:1209))347.7100CH31015.7509.4 575.4168.5m/zOO318.0CH3OHHO%HO509.7%HO510.0OH318.7319.3O9001000501.7510.8349.3141.4687.0366.7163.6 265.8349.8531.6447.4m/z200300400500O510.6501.3502.9319.7231.7OHOHOH348.7319.0142.2OO318.40100m/z14001: Scan ES+5.13e6CH360070080011001200130014000100532.8646.4812.6910.2800900m/z20030040050060070010001100120013001400В фракции №4 присутствуют 3 пика с временами удерживания 18.53,18.73 и 19.11 мин, которые отсутствуют в других фракциях и могут иметьструктуры3’,3-Dimethylquercetin(былобнаруженлитературным данным), Rhamnazin и Centaureidin:ранеесогласно164N4N4N4MR-RUDN-270717-1 22235 (18.531) Cm (22178:22291-21980:22069)2: Diode Array1.806e-2341.8219.81.8e-2MR-RUDN-270717-1 22479 (18.735) Cm (22420:22538-(22618:22678+22347:22376))254.82: Diode Array3.579e-2OH3 C2.5e-2OHOOO6.0e-3OHOCH3OHOO5.0e-35.0e-3m/z8009001000110012001300329.1100CH314001: Scan ES1.53e6O1.0e-2OHOOHO1.0e-22.0e-3OH255.81.5e-21.5e-24.0e-30.0100200300400500600700MR-RUDN-270717-2 2189 (18.563) Cm (2181:2194-2163:2173)CH3O351.8OOAU8.0e-32.0e-2H3 C2.0e-21.0e-2Centaureidin2.5e-2AU1.2e-22: Diode Array2.981e-2219.8CH3219.8OH1.4e-2MR-RUDN-270717-1 22925 (19.106) Cm (22869:22990-22607:22777)Rhamnazin; Rhamnacine; 3',7-DimethylquercetinOH269.83.0e-2AU355.83.5e-23,7-Di-O-methylquercetin1.6e-2OH H3C0.0100200300400500600700800MR-RUDN-270717-2 2211 (18.750) Cm (2205:2219-(2224:2233+2194:2200))m/z9001000110012001300329.110014001: Scan ES2.52e60.0100200300400500600700800MR-RUDN-270717-2 2256 (19.131) Cm (2246:2261-(2264:2282+2223:2239))100900100011001200130080090010001100120013008009001000110012001300359.1249.0m/z14001: Scan ES1.44e6249.5329.5329.5%%%359.6329.8265.2330.0265.5168.9169.4328.4330.2330.8397.5440.7168.81261.60100200300400500600700800MR-RUDN-270717-1 2186 (18.537) Cm (2184:2196-(2176:2182+2200:2203))9001000110012001300331.7100m/z14001: Scan ES+1.29e7317.2397.0281.60100200300400500600700800MR-RUDN-270717-1 2212 (18.757) Cm (2207:2220-(2223:2234+2199:2202))9001000110012001300331.8100360.0361.0178.8659.5m/z14001: Scan ES+2.25e7521.4522.4515.4583.2427.0631.30100200300400500600700MR-RUDN-270717-1 2256 (19.130) Cm (2248:2263-2219:2245)788.1 805.5361.8100m/z14001: Scan ES+1.43e7%%%332.1273.9233.7332.6332.6333.0362.7187.9333.3187.6289.7300400363.5383.7353.8142.7158.5m/z200289.8290.2333.7353.60100271.6135.4500600700800900100011001200130014000100m/z200300400500600MW80090010001100120013001400Средние значенияAverName700M+ fragm/z2003004005006007001400Площадь пика на ТАС-хроматограммах* фракцииUV-max, nmtR, min13487.742.23E+108.59E+10234Linariifolioside654Quercetin 3-glucuronide4783033558.09Hyperoside4643033548.21Luteolin 7-O-glucuronide4622873358.29Quercetagetin 3'-methyl ether 3-glucoside4943333528.528.85E+09isorhamnetin-3-O-glucoside4783173459.932.12E+10Quercetagetin 3',4'-dimethyl-3-O-glucoside50834735510.301.76E+10Quercetagetin 3'-methyl ether332NA37214.023.21E+101.58E+103-Methylquercetin316NA34614.162.97E+101.68E+10Nepetin316NA35715.126.95E+105.60E+10Tomentin; 3,7-Dimethylquercetagetin346NA35815.393.59E+103.88E+10Hispidulin300NA33516.805.05E+101.02E+113’,3-Dimethylquercetin330NA34218.531.74E+10Rhamnazin; Rhamnacine; 3',7-Dimethylquercetin330NA35618.733.14E+10Centaureidin360NA35219.11Rhamnetin316NA36920.66SummNA01003.75E+103.04E+101.61E+101.39E+110.00E+002.01E+103.23E+11Таким образом, наибольшее количество флавонов и флавоноловсодержится в фракции №3, а в фракции № 2 они не обнаружены.4.