Table 1. Summary of Chemical Constituents About Supercritical CO2 Fluid Extraction from CRS by Ultra-HPLC Combined with Q-Exactive Orbitrap Tandem Mass Spectrometry.
| no. | tR (min) | [M + H]+ (m/z) | fragment ions (m/z) | compound formula | identification |
|---|---|---|---|---|---|
| 1 | 0.03 | 195.0875 | 177.0912, 167.0847, 153.0544, 146.9612, 138.0662, 135.0442, 123.0432, 114.6795, 110.0716, 107.0856, 89.0602, 79.0550, 69.0455, 58.0659 | C8H10N4O2 | caffeine |
| 2 | 0.70 | 124.0394 | 119.0366, 106.0655, 101.0255, 96.0448, 90.0198, 80.0501, 78.0343, 68.0503, 62.9905, 53.0393 | C6H5NO2 | nicotinic acid |
| 3 | 0.82 | 123.0553 | 118.0349, 108.9585, 105.0374, 100.0247, 96.0448, 90.5265, 88.0236, 86.0262, 80.0500, 76.5157, 67.5105, 62.9906, 56.9656, 53.0392 | C6H6N2O | nicotinamide |
| 4 | 1.92 | 156.1019 | 138.0913, 122.8464, 113.0840, 110.0967, 108.0810, 96.0812, 88.0762, 86.0606, 84.0451, 82.0657, 71.0498, 69.0342, 67.0548, 53.0394 | unknown | unknown |
| 5 | 2.40 | 137.1073 | 122.0837, 96.0811, 88.2350, 80.0502, 69.0706, 60.5088, 55.0550 | C8H12N2 | tetramethylpyrazine |
| 6 | 2.91 | 153.0546 | 144.6615, 134.0600, 125.0597, 122.4801, 113.0483, 111.0442, 107.0494, 97.0652, 93.0339, 88.9528, 79.0548, 70.9424, 65.0393, 63.0239 | C8H8O3 | vanillin |
| 7 | 3.01 | 183.0652 | 173.9848, 165.0906, 159.9690, 155.0702, 145.9897, 140.0467, 131.9742, 123.0442, 113.9639, 105.0450, 98.9845, 95.0495, 90.9481, 86.9537, 81.0341, 72.9378, 67.0550, 65.0393, 56.9430 | C9H10O4 | 3,5-dimethoxy-4-hydroxybenzaldehyde |
| 8 | 4.21 | 207.0652 | 201.9320, 192.0416, 179.0704, 175.0391, 163.0390, 151.0754, 148.0517, 121.0650, 107.0495, 91.0547, 79.0548, 67.0548 | C11H10O4 | scoparone |
| 9 | 4.41 | 147.0440 | 137.9799, 129.0700, 123.9644, 119.0857, 105.9538, 103.0545, 95.0496, 91.0547, 84.0813, 73.0845, 64.9280, 53.0393 | C9H6O2 | coumarin |
| 10 | 6.61 | 133.0648 | 119.9576, 117.9598, 115.0544, 109.5154, 105.0701, 103.0546, 98.0076, 96.0099, 91.0547, 89.0023, 83.8491, 79.0548, 77.0390, 72.0814, 65.0394, 58.0336 | C9H8O | cinnamaldehyde |
| 11 | 7.24 | 303.0859 | 285.0751, 262.1411, 243.0657, 219.0645, 201.0540, 185.0447, 177.0546, 163.0389, 153.0182, 135.0441, 117.0337, 111.0080, 89.0390, 67.0185 | C16H14O6 | hesperitin |
| 12 | 8.13 | 223.0964 | 214.0120, 205.0857, 199.9964, 186.0551, 177.0546, 163.0389, 149.0597, 145.0284, 135.0441, 121.0650, 117.0337, 107.0859, 93.0703, 89.0391, 79.0548, 67.0550 | C12H14O4 | ethyl ferulate |
| 13 | 8.99 | 471.2012 | 453.1918, 425.1955, 409.2001, 383.2280, 367.1904, 339.1947, 321.1846, 279.1379, 225.0913, 213.0910, 187.0753, 161.0597, 133.0648, 105.0702, 95.0132, 79.0548 | C26H30O8 | limonina |
| 14 | 9.07 | 151.1117 | 146.0297, 139.0752, 128.0193, 123.0806, 121.0650, 113.9638, 109.0650, 105.0700, 95.0859, 87.0045, 81.0704, 79.0547, 67.0550, 65.0393, 55.0549 | C10H14O | 2-adamantanone |
| 15 | 9.41 | 245.1170 | 227.1066, 217.1214, 203.1063, 199.1116, 189.0544, 171.1166, 156.0934, 145.0647, 131.0492, 119.0857, 105.0702, 95.0495, 81.0341, 76.9062, 67.0550, 55.0186 | C15H16O3 | linderalactone |
| 16 | 9.63 | 403.1385 | 388.1148, 373.0914, 358.0676, 327.0854, 301.0701, 284.0666, 258.0519, 229.0339, 211.0235, 193.0125, 183.0287, 165.0546, 1227.0389, 99.0443, 69.0341 | C21H22O8 | nobiletina |
| 17 | 9.76 | 287.0910 | 269.0804, 245.0814, 203.0699, 179.0332, 171.0286, 161.0596, 153.0181, 133.0647, 118.0414, 103.0547, 67.0185 | C16H14O5 | isosakuranetin |
| 18 | 9.78 | 343.1173 | 327.0856, 313.0701, 299.0909, 282.0881, 267.0650, 239.0699, 199.0233, 171.0285, 153.0181, 133.0647, 122.0363, 86.0967, 69.0339 | C19H18O6 | 6-demethoxytangeretin |
| 19 | 9.89 | 515.2271 | 469.2221, 455.2037, 419.1846, 411.2158, 393.2051, 349.1804, 321.1849, 279.1374, 243.0992, 215.1061, 187.0752, 161.0596, 133.0647, 95.0131, 81.0340 | unknown | unknown |
| 20 | 10.16 | 433.1488 | 418.1254, 403.1019, 385.0911, 345.0599, 317.0650, 289.0700, 255.0640, 211.0230, 183.0290, 165.0544, 149.0235, 127.0387, 94.0416, 70.9067 | C22H24O9 | 3,5,6,7,8,3′,4′-heptamethoxyflavonea |
| 21 | 10.31 | 137.0596 | 122.0734, 119.0493, 116.5949, 109.0650, 107.0493, 105.0451, 95.0495, 93.0703, 91.0547, 81.0705, 79.0549, 67.0549, 54.4142, 53.0394 | C8H8O2 | p-anisaldehyde |
| 22 | 10.53 | 231.1378 | 213.1274, 189.0910, 185.1324, 175.0754, 163.0752, 143.0855, 135.0442, 119.0857, 105.0702, 91.0547, 69.0706, 55.0550 | C15H18O2 | atractylenolide-I |
| 23 | 10.57 | 373.1280 | 358.1041, 343.0809, 328.0570, 297.0753, 283.0602, 271.0599, 254.0569, 229.0319, 211.0235, 193.0132, 183.0287, 168.0051, 135.0440, 99.0444, 68.9978 | C20H20O7 | tangeretina |
| 24 | 10.76 | 455.2060 | 437.1934, 419.1848, 409.2013, 391.1895, 359.1282, 349.1430, 315.1386, 303.1373, 263.068, 235.1124, 197.0964, 175.0754, 161.0596, 133.0648, 105.0702, 95.0132, 79.0548, 67.0550 | C26H30O7 | obacunone |
| 25 | 10.82 | 183.0804 | 173.9850, 159.9689, 141.9586, 131.9742, 127.9794, 118.9675, 113.9638, 105.0338, 100.9570, 95.0495, 81.0705, 72.9378, 67.0549, 59.9310, 56.9430 | C13H10O | atractylodin |
| 26 | 11.10 | 389.1227 | 374.0992, 359.0757, 341.0652, 331.0807, 316.0574, 285.0761, 260.0672, 227.0544, 215.0184, 197.0080, 187.0235, 169.0130, 163.0752, 148.0518, 113.0237, 85.0291, 55.0185 | C20H20O8 | 5-hydroxy-6,7,8,3′,4′-pentamethoxyflavonea |
| 27 | 11.72 | 191.1064 | 173.0959, 163.1115, 149.0596, 145.1010, 135.0438, 130.0778, 121.0651, 117.0700, 105.0701, 93.0702, 91.0546, 81.0706, 79.0548, 69.0704, 67.0549, 55.0550 | C12H14O2 | ligustilides |
| 28 | 11.91 | 189.0907 | 171.0802, 166.0290, 156.0927, 153.0697, 143.0854, 133.1015, 128.0620, 125.0960, 117.0698, 105.0701, 97.1014, 91.0547, 83.0860, 67.0550, 55.0550 | C12H12O2 | N-butylidenephthalide |
| 29 | 12.52 | 233.1533 | 215.1428, 205.1582, 197.1323, 187.1479, 177.0908, 173.0961, 159.0803, 151.0752, 145.1010, 131.0854, 119.0857, 105.0701, 95.0859, 81.0704, 67.0549 | C15H20O2 | atractylenolide-II |
| 30 | 16.07 | 295.2263 | 277.2158, 259.2050, 241.1943, 223.1689, 205.1582, 187.1482, 173.1321, 161.1323, 147.1165, 135.1167, 121.1012, 107.0858, 95.0859, 81.0704, 67.0549 | Unknown | unknown |
| 31 | 17.98 | 324.2893 | 307.2624, 263.2367, 245.2264, 161.1329, 133.1013, 109.1013, 95.0858, 67.0549, 62.0608 | Unknown | unknown |
| 32 | 18.79 | 307.2627 | 261.2208, 243.2102, 233.2252, 219.2103, 187.1481, 173.1322, 145.1009, 137.1322, 123.1168, 109.1013, 95.0858, 81.0704, 67.0549 | C20H34O2 | linolenic acid ethyl ester |
a
Further confirmation in comparison with standard compound.