Fingerprint and Identification of Chemical Constituents of the Extract of Fructus Ligustri Lucidi-Ecliptae Herba
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摘要:
目的 建立女贞子-墨旱莲药对提取物的HPLC指纹图谱以控制其质量, 并对提取物中所含有的化学成分进行结构鉴定。 方法 采用HPLC法, 固定相为ZORBAX Extend C18色谱柱(4.6 mm×250 mm, 5 μm), 流动相为乙腈-体积分数为0.1%甲酸溶液梯度洗脱, 流速为1.0 mL·min-1, 检测波长为265 nm, 柱温为35 ℃, 进样量为10 μL; 建立15批不同产地女贞子-墨旱莲药对提取物的HPLC指纹图谱, 对其进行相似度评价、聚类分析和正交偏最小二乘方判别分析; 采用超高效液相色谱-静电场轨道阱高分辨质谱(UPLC-Q-Exactive Orbitrap MS)联用技术, 分别在正、负离子扫描模式下对提取中的化学成分进行检测, 基于高分辨质谱一级和二级数据进行结构鉴定。 结果 由不同产地药材随机组合的15批女贞子-墨旱莲药对提取物的相似度介于0.865~0.992之间, 药对指纹图谱中共确定了16个共有峰, 指认了其中7个色谱峰; 液质联用共检测到55个化合物, 采用对照品准确鉴定了7个成分的化学结构, 并推测了其它48个化合物的可能化学结构。 结论 建立的指纹图谱方法简便可靠, 重复性好, 可用于女贞子-墨旱莲药对提取物的质量控制研究; UPLC-Q-Exactive Orbitrap MS联用技术可实现对女贞子-墨旱莲药对提取物中化合物的结构鉴定, 为其后续研究奠定了基础。 Abstract:OBJECTIVE To establish high performance liquid chromatography (HPLC) fingerprints of the extract of Fructus Ligustri Lucidi-Ecliptae Herba and to identify the structure of its chemical constituents. METHODS The chromatographic separation was performed on ZORBAX Extend C18 (250 mm×4.6 mm, 5 μm) column with the mobile phase consisting of acetonitrile and 0.1% formic acid solution in gradient elution mode at a flow rate of 1.0 mL·min-1. The optimum column temperature was set at 35 ℃, the detection wavelength was 265 nm, and the injection volume was 10 μL. The HPLC fingerprints of 15 batches of herb pair from different origins were established. Then, similarity evaluation, cluster analysis, and orthogonal partial least squares discriminant analysis were carried out. The chemical structures of the constituents of the herb pair were identified based on the high-resolution mass spectrometry utilizing the UPLC-Q-Exactive Orbitrap MS in positive and negative-ion modes. RESULTS As a result, the similarity of the 15 batches of samples varied from 0.865 to 0.992. A total of 16 common peaks were identified in the fingerprints, and 7 of them were identified by comparision with the reference substances. Furthermore, 55 chemical compounds were detected, and 7 of them were accurately identified based on the reference substances, and the chemical structures of the rest 48 components were temporarily speculated. CONCLUSION The fingerprint method established in this study is simple, reliable, and reproducible, and can be further used for the quality control of Fructus Ligustri Lucidi-Ecliptae Herba herb pair. The developed UPLC-Q-Exactive Orbitrap MS method can be applied to identify the structures of chemical constituents in this herb pair and lay a foundation for further research. -
Key words:
- Fructus Ligustri Lucidi /
- Ecliptae Herba /
- fingerprint /
- UPLC /
- Q-Exactive Orbitrap MS /
- chemical constituents
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图 1 15批女贞子-墨旱莲药对药材HPLC指纹图谱叠加图
Figure 1. HPLC fingerprints of 15 batches of herb pair of Fructus Ligustri Lucidi and Ecliptae Herba
图 2 对照品溶液色谱图(A)及供试品溶液色谱图(B)
注:5号峰为芦丁; 7号峰为木犀草苷; 9号峰为特女贞苷; 11号峰为木犀草素; 12号峰为女贞苷G13;13号峰为蟛蜞菊内酯; 16号峰为芹菜素
Figure 2. HPLC of mixed control solution(A) and herb pair of Fructus Ligustri Lucidi and Ecliptae Herba(B)
图 3 女贞子-墨旱莲药对样品聚类分析树状图
Figure 3. Dendrogram of hierarchical cluster analysis of 15 batches of herb pair of Fructus Ligustri Lucidi and Ecliptae Herba
图 4 15批次女贞子-墨旱莲药对样品的OPLS-DA得分图
Figure 4. OPLS-DA score plots of 15 batches of herb pair of Fructus Ligustri Lucidi and Ecliptae Herba
图 5 各批次女贞子-墨旱莲样品16个共有峰的VIP值
注:X1~X16.1~16号峰
Figure 5. VIP values of 16 common peaks in 15 batches of herb pair of Fructus Ligustri Lucidi and Ecliptae Herba
图 6 女贞子-墨旱莲药对供试品溶液在正离子模式下的总离子流色谱图
Figure 6. TIC of herb pair of Fructus Ligustri Lucidi-Ecliptae Herba in positive ion mode
图 7 女贞子-墨旱莲药对供试品溶液在负离子模式下的总离子流色谱图
Figure 7. TIC of herb pair of Fructus Ligustri Lucidi-Ecliptae Herba in negative ion mode
图 12 特女贞苷二级质谱图及裂解方式
Figure 12. Fragment ion spectrum and cleavage mode of Specnuezhenide
图 14 蟛蜞菊内酯二级质谱图及裂解方式
Figure 14. Fragment ion spectrum and cleavage mode of Wedelolactone
图 15 异绿原酸C二级质谱图及裂解方式
Figure 15. Fragment ion spectrum and cleavage mode of Isochlorogenic acid C
图 16 松果菊苷二级质谱图及裂解方式
Figure 16. Fragment ion spectrum and cleavage mode of Echinacoside
图 18 D-(+)-色氨酸二级质谱图及裂解方式
Figure 18. Fragment ion spectrum and cleavage mode of D-(+)tryptophan
表 1 女贞子和墨旱莲饮片来源及批号信息
Table 1. The origins and batch number of herbal pieces of Fructus Ligustri Lucidi and Ecliptae Herba
女贞子 墨旱莲 产地 批号 产地 批号 江苏省 C021220502 江苏省 20220802442 浙江省 201201 河南省 240220902 四川省 200801 河南省 220901 广东省 211101 河南省 221001 河南省 220801 广东省 2209169 河南省 2210012 广东省 211101 山东省 220601 安徽省 220301 广西省 220802361 安徽省 220701 广西省 221200711 湖南省 220901 广西省 210901 四川省 221001 
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表 2 女贞子和墨旱莲15批物质基准对应的饮片批次
Table 2. 15 batches of Fructus Ligustri Lucidi and Ecliptae Herba substance benchmarks corresponding to the batches of decoction pieces
批号 女贞子 墨旱莲 S1 220802361 220701 S2 221200711 221001 S3 210901 220901 S4 220401 220701 S5 220601 220701 S6 220801 211101 S7 220401 2209169 S8 C021220502 240220902 S9 201201 20220802442 S10 201201 2209169 S11 210901 220301 S12 2210012 221001 S13 210901 20220802442 S14 211101 220301 S15 220802361 220901
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表 3 不同批次女贞子-墨旱莲药对的相似度评价结果
Table 3. Similarities of 15 batches of herb pair of Fructus Ligustri Lucidi and Ecliptae Herba
编号 相似度 编号 相似度 编号 相似度 编号 相似度 编号 相似度 1 0.959 4 0.979 7 0.986 10 0.982 13 0.955 2 0.985 5 0.955 8 0.990 11 0.991 14 0.865 3 0.991 6 0.964 9 0.991 12 0.953 15 0.992
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表 4 UPLC-Q-Exactive Orbitrap MS鉴定的女贞子-墨旱莲药对提取物中的化学成分
Table 4. The chemical constituents in herb pair of Fructus Ligustri Lucidi-Ecliptae Herba identified by UPLC-Q-Exactive Orbitrap MS
峰号 tR/min [M+H]+ [M+H]- 主要碎片离子 分子式 化合物 来源 类别 理论值 实际值 误差 理论值 实际值 误差 1 2.95 - - - 451.109 59 451.109 33 1.46 (-)151.039 36, 123.044 14 C17H24O14 女贞子酸 Nuezhenidic acid N 环烯醚萜类 2 3.15 355.102 05 355.102 34 -0.61 353.088 17 353.087 80 -0.32 (-)353.087 77, 161.023 47 C16H18O9 新绿原酸 Cryptochlorogenic acid M 酚酸类 3 3.67 301.128 48 301.128 17 -0.02 299.113 71 299.113 63 0.79 (-)119.049 03 C14H20O7 红景天苷 Salidroside N 苯乙醇苷 4 3.69 205.082 26 205.082 60 -0.01 203.082 26 203.082 60 3.19 (-)116.049 43, 142.065 37, 159.092 75, 203.082 86 C11H12N2O2 D-(+)色氨酸 D-(+)tryptophan M 氨基酸类 5 4.39 433.169 95 433.170 43 3.65 431.168 70 431.170 44 -0.11 (-)149.045 06, 119.048 96 C19H28O11 - Osmanthuside H N 苯乙醇苷 6 4.66 355.102 05 355.102 36 -0.61 353.088 32 353.087 80 -0.66 (-)353.087 77, 191.055 50, 179.034 06, 173.044 77, 161.023 47, 135.044 02 C16H18O9 绿原酸 Chlorogenic acid M 酚酸类 7 6.04 - - - 583.205 26 583.203 23 -0.79 (-)537.256 10 C27H36O14 女贞果苷C Lucidumoside C N 环烯醚萜类 8 6.66 303.049 87 303.049 93 -0.71 301.035 74 301.035 37 1.19 (-)301.036 04, 257.044 01 C15H10O7 桑色素 Morin M 黄酮类 9 7.27 319.043 46 319.044 84 -3.87 317.030 09 317.030 29 -0.63 (+)273.038 51, 181.012 97, 153.018 16, 121.028 63 C15H10O8 杨梅素 Myricetin M 黄酮类 10 7.31 787.264 95 787.265 52 -1.26 785.251 89 785.252 44 1.17 (-)785.252 44, 623.221 25, 221.901 37, 161.023 54 C35H46O20 松果菊苷 Echinacoside N 苯乙醇苷 11 8.61 379.138 61 379.138 74 -0.35 377.145 66 377.124 19 0.26 (-)197.081 42, 153.091 16 C19H22O8 橄榄苦苷元 Oleuropein aglycon N 环烯醚萜类 12 8.70 - - - 395.009 58 395.007 84 2.40 (-)255.030 29, 299.020 32, 271.025 76, 221.440 16 C16H12O10S 水蓼素 Persicarin M 黄酮类 13 8.77* 611.160 40 611.160 66 -0.83 609.146 40 609.146 11 -0.37 (-)273.037 76, 301.034 33, 151.002 66, 255.031 32 C27H30O16 芦丁 Rutin N 黄酮类 14 9.09 - - - 555.183 90 555.186 48 1.11 (-)223.060 64, 157.039 17, 123.044 05 C25H32O14 - Ligustaloside A N 环烯醚萜类 15 9.18 465.100 95 465.102 75 -0.35 463.086 49 463.088 20 0.87 (-)391.035 64, 269.008 91, 151.002 78 C21H20O12 异槲皮苷 Isoquercitrin M 黄酮类 16 9.47* 449.107 48 449.107 83 -1.06 447.093 28 447.093 81 0.31 (-)327.051 27, 285.040 50, 146.959 55 C21H20O11 木犀草苷 Luteoloside M, N 黄酮类 17 9.69 571.163 21 571.165 75 -0.92 569.153 08 569.151 19 1.05 (-)209.045 01, 177.018 74, 165.055 51, 123.044 07 C25H30O15 橄榄苦苷酸 Oleuropeinic acid N 环烯醚萜类 18 9.76* 449.107 48 449.107 83 -0.79 447.093 81 447.093 28 -0.09 (-)285.039 73, 284.032 56, 256.037 87, 174.955 51, 146.959 79 C21H20O11 槲皮苷 Quercitrin M, N 黄酮类 19 9.97 - - - 701.226 81 701.229 84 0.85 (-)539.177 92, 315.109 44, 135.044 24, 101.022 90 C31H42O18 新女贞苷 Neonuezhenide N 环烯醚萜类 20 10.69 625.211 12 625.212 69 -2.03 623.210 14 623.212 70 0.55 (-)623.198 85, 461.165 65, 315.950 96 C29H36O15 毛蕊花糖苷 Acteoside N 苯乙醇苷 21 10.73* 687.245 73 687.249 47 3.09 685.250 43 685.249 48 0.62 (-)523.181 88, 453.141 14, 421.153 05, 299.113 83, 223.061 51 C31H42O17 特女贞苷 Specnuezhenide N 环烯醚萜类 22 11.58 517.133 79 517.134 05 -0.51 515.120 06 515.119 49 0.45 (-)173.044 74, 146.960 40 C25H24O12 异绿原酸B Isochlorogenic acid B M 酚酸类 23 11.65 317.065 22 317.065 57 -1.15 315.051 09 315.051 02 0.48 (-)300.027 74, 151.002 93 C16H12O7 异鼠李素 Isorhamnetin M 黄酮类 24 11.71 - - - 299.034 61 299.034 28 0.77 (-)271.025 15, 243.030 03, 201.018 42, 183.044 56 C15H8O7 去甲基蟛蜞菊内酯 Demethylwedelolactone M 香豆素类 25 11.78 301.033 94 301.034 27 -0.63 299.034 21 299.034 28 -0.23 (-)191.040 10, 271.024 87 C15H8O7 异去甲蟛蜞菊内酯 Isodemethylwedelolacton M 香豆素类 26 11.98 517.133 79 517.134 05 -0.27 515.120 12 515.119 49 -0.25 (-)353.088 53, 179.034 21, 173.044 75 C25H24O12 异绿原酸A Isochlorogenic acid A M 酚酸类 27 12.00 305.065 43 305.065 57 -0.49 303.050 96 303.051 03 2.11 (-)149.996 16, 121.028 75 C15H12O7 花旗松素 Taxifolin N 黄酮类 28 12.38 - - - 461.147 58 461.145 32 1.06 (-)461.108 8, 299.053 50 C23H26O10 - Neosyringalide N 苯乙醇苷 29 12.56 - - - 723.211 06 723.214 18 -2.74 (-)525.163 27, 455.117 25, 300.028 41 C33H40O18 女贞苷 Ligustroflavone N 环烯醚萜类 30 12.73 687.248 96 687.249 47 -0.75 685.250 43 687.249 48 0.62 (-)523.180 42, 453.142 43, 299.113 71, 119.048 92 C31H42O17 女贞次苷 1''-O-β-D-glucosylformoside N 环烯醚萜类 31 12.84 555.170 47 555.170 83 -1.19 553.155 33 553.156 28 -0.29 (-)209.045 52, 177.018 57, 151.039 66, 101.023 22 C25H30O14 女贞苷酸 Ligustrosidic acid N 环烯醚萜类 32 12.96 433.112 67 433.112 92 -0.58 431.096 95 431.098 37 0.75 (-)431.098 51, 269.043 95, 130.982 60 C21H20O10 芹菜素-7-O-β-D-葡萄糖苷 Cosmosiin N 黄酮类 33 14.05 687.249 33 687.249 47 -0.21 685.249 27 685.249 48 0.62 (-)453.140 20, 299.114 14, 223.061 57, 119.049 03 C31H42O17 异女贞苷 Isonuezhenide N 环烯醚萜类 34 14.08 541.191 59 541.191 57 -0.19 539.177 80 539.177 01 1.44 (-)377.124 11, 307.082 52, 149.023 7 C25H32O13 橄榄苦苷 Oleuropein N 环烯醚萜类 35 14.32 188.070 48 188.070 60 -0.66 - - - (+)170.059 80, 146.059 89 C11H9NO2 反式-3-吲哚丙烯酸 3-Indoleacrylic acid M 脂肪酸 36 14.68 367.011 87 367.011 82 0.12 365.011 93 365.011 83 0.77 (-)285.040 86 C15H10O9S 木犀草素-7-硫酸盐 Luteolin 7-sulfate M 黄酮类 37 14.79 517.134 03 517.134 05 -0.04 515.119 87 515.119 39 0.84 (-)353.088 23, 191.055 30, 179.034 41, 173.044 72 C25H24O12 异绿原酸C Isochlorogenic acid C M 酚酸类 38 16.59 - - - 537.199 16 537.197 75 1.82 (-)375.070 19 C26H34O12 - Ligustaloside B N 环烯醚萜类 39 18.77 287.054 96 287.055 01 -0.50 285.040 99 285.040 46 1.83 (+)287.054 72, 269.043 79, 241.049 10, 213.054 52, 153.018 14 C15H10O6 野黄芩素 Scutellarein M 黄酮类 40 19.51 289.070 62 289.070 66 -0.16 287.057 34 287.056 11 1.63 (-)287.150 3, 269.139 01 C15H12O6 圣草素 Eriodictyol N 黄酮类 41 21.26 303.049 87 303.049 93 -0.01 301.035 68 301.035 37 2.01 (-)301.036 29, 245.046 60 C15H10O7 槲皮素 Quercetin N 黄酮类 42 21.40* 287.054 75 287.055 11 -0.71 285.054 75 285.055 01 1.51 (-)273.041 20, 151.002 87, 257.044 80, 241.049 91, 151.002 99, 133.028 49 C15H10O6 木犀草素 Luteolin M, N 黄酮类 43 21.63 - - - 523.183 65 523.182 10 1.45 (-)291.089 02, 101.023 15 C25H32O12 女贞苷 Ligustroside N 环烯醚萜类 44 23.30* 315.049 19 315.049 92 -2.52 313.036 16 313.035 38 0.56 (+)315.049 53, 297.039 06, 271.05936, 269.04422, 287.054 87, 243.064 79 C16H10O7 蟛蜞菊内酯 Wedelolactone M 香豆素类 45 25.53 1 073.370 48 1 073.370 77 -0.27 1 071.368 29 1 071.370 77 0.55 (-)685.237 18, 523.182 98, 299.114 17 C48H64O27 - Oleonuezhenide N 环烯醚萜类 46 26.07* 271.262 73 271.060 09 -0.49 269.046 14 269.045 55 1.87 (-)269.046 08, 225.055 53, 183.044 59 C15H10O5 芹菜素 Apigenin M, N 黄酮类 47 26.35* 1 073.373 17 1 073.370 77 2.23 1 071.368 29 1 071.370 77 0.78 (-)909.295 65, 839.263 61, 685.234 62, 532.184 63, 403.124 15 C48H64O27 女贞苷G13 GL3 N 环烯醚萜类 48 26.48 301.070 34 301.034 28 -0.35 299.056 76 299.056 11 2.17 (-)284.033 08, 255.030 29 C16H12O6 香叶木素 Diosmetin M 黄酮类 49 28.19 331.247 62 331.247 90 -0.84 329.234 01 329.233 34 2.01 (-)201.113 14, 171.101 90 C18H34O5 - Pinellic acid M 脂肪酸 50 29.67 635.415 16 635.415 35 -0.31 633.400 80 633.405 89 1.27 (+)455.351 56, 191.179 31 C36H58O9 旱莲苷A Ecliptasaponin A M 三萜类 51 33.19 375.107 09 375.107 44 -0.95 373.091 28 373.092 89 2.14 (-)135.080 64, 181.897 00 C19H18O8 黄芩黄酮Ⅱ Skullcapflavone Ⅱ M 黄酮类 52 37.73 311.221 41 311.221 68 -0.90 309.207 86 309.207 13 2.13 (+)293.210 36, 155.106 35 C18H30O4 - Porrigenic acid M 脂肪酸 53 44.22 471.347 05 471.346 88 -0.24 469.332 98 469.332 33 1.37 (+)471.346 71, 303.122 65, 208.178 09 C30 H46O4 18-β-甘草次酸 Glycyrrhetinic acid M 三萜类 54 48.28 457.367 62 457.366 73 -4.34 455.353 06 455.353 55 1.04 (-)453.353 79, 407.337 86 C30H48O3 齐墩果酸 Oleanolic acid N 三萜类 55 51.16 - - - 279.233 73 279.232 95 0.72 (-)279.233 49 C18H32O2 亚油酸 Linoleic acid M, N 脂肪酸 注:*为对照品指认；M.墨旱莲；N.女贞子。
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