桂枝茯苓胶囊中三萜酸类成分的UPLC/Q-TOF-MS指纹图谱研究
|
摘要
目的建立桂枝茯苓胶囊(GFC)中三萜酸类成分UPLC/Q-TOF-MS指纹图谱方法,为评价GFC的质量提供新方法。方法采用UPLC分离三萜酸类成分,用Q-TOF-MS检测,建立UPLC/Q-TOF-MS指纹图谱。结果得到灵敏度、选择性和专属性良好的GFC中三萜酸类成分UPLC/Q-TOF-MS指纹图谱,确定了26个共有峰,其中3、5～18、20、23、24共18个峰来自于茯苓,2号峰来自于白芍和牡丹皮,4号峰来自于茯苓、牡丹皮、白芍、桂枝,19号峰来自于牡丹皮、白芍和桂枝,21号峰来自于牡丹皮和白芍,22、25号峰来自于茯苓、牡丹皮、桃仁、白芍、桂枝,26号峰来自于桂枝、白芍、桃仁。10批GFC指纹图谱相似度在0.90以上。UPLC-Q-TOF-MS共鉴定出16个成分,分别为16α-羟基松苓新酸、16α-羟基-栓菌酸、3-酮基-6,16α-二羟基-羊毛甾-7,9(11),24-三烯-21酸、去氢土莫酸、土莫酸、3-酮基-6,16α-二羟基-羊毛甾-8,24-二烯-21酸、依布里酸、猪苓酸C、3-表去氢土莫酸、3-O-乙酰基-16α-羟基松苓新酸、3-表去氢茯苓酸、3-O-乙酰基-16α-羟基-栓菌酸、去氢茯苓酸、茯苓酸、松苓新酸、去氢齿孔酸。结论该方法准确、快速,具有较好的精密度、重复性和稳定性,适用于GFC的质量控制。
Objective To construct the fingerprint of the triterpenoic acid in Guizhi Fuling Capsule(GFC) by UPLC/Q-TOF-MS, and give a new method for its quality control. Methods The triterpenoic acid were isolated by UPLC and detected by Q-TOF-MS. The established fingerprint was an atlas of UPLC/Q-TOF-MS. Results The UPLC/Q-TOF-MS fingerprints of triterpenoids in GFC were established, which preserved high precision, selectivity, and specificity. A total of 26 common peaks were selected as the fingerprint peaks of GFC, of which a total of 18 mutual peaks(3, 5—18, 20, 23, and 24) from Poria, peak 2 was from Paeoniae Radix Alba and Moutan Cortex. Peak 4 was from Poria, Moutan Cortex, Paeoniae Radix Alba, and Cinnamomi Ramulus. Peak 19 was from Moutan Cortex, Paeoniae Radix Alba, and Cinnamomi Ramulus, peak 21 was from Moutan Cortex and Paeoniae Radix Alba, peaks 22 and 25 were from Poria, Moutan Cortex, Persicae Semen, Paeoniae Radix Alba, and Cinnamomi Ramulus, peak 26 was from Cinnamomi Ramulus, Paeoniae Radix Alba, and Persicae Semen. The similarity among the 10 batches of GFC was above 0.90. The results of validation met technical requirement of fingerprints. Sixteen chemical components were identified by UPLC-Q-TOF-MS, which were 16α-hydroxydehydrotrametenolic acid, 16α-hydroxychalcic acid, 3-oxo-6,16α-dihydroxy-lanosta-7,9(11),24(31)-trien-21-oic acid, dehydrotumulosic acid, tumulosic acid, 3-oxo-6,16α-dihydroxy-lanosta-8,24-diene-21-oic acid, eburicoic acid, polyporenic acid C, 3-epidehydrotumulosic acid, 3-O-acetyl-16α-hydroxydehydrotrametenolic acid, 3-epidehydropachymic acid, 3-O-acetyl-16α-hydroxyplugymic acid, dehydropachymic acid, pachymic acid, dehydrotrametenolic acid, and dehydroeburicoic acid. ConclusionThe method is rapid, accurate, and has desirable precision, reproducibility, and stability, which could be applied to the quality control of GFC.
Objective To construct the fingerprint of the triterpenoic acid in Guizhi Fuling Capsule(GFC) by UPLC/Q-TOF-MS, and give a new method for its quality control. Methods The triterpenoic acid were isolated by UPLC and detected by Q-TOF-MS. The established fingerprint was an atlas of UPLC/Q-TOF-MS. Results The UPLC/Q-TOF-MS fingerprints of triterpenoids in GFC were established, which preserved high precision, selectivity, and specificity. A total of 26 common peaks were selected as the fingerprint peaks of GFC, of which a total of 18 mutual peaks(3, 5—18, 20, 23, and 24) from Poria, peak 2 was from Paeoniae Radix Alba and Moutan Cortex. Peak 4 was from Poria, Moutan Cortex, Paeoniae Radix Alba, and Cinnamomi Ramulus. Peak 19 was from Moutan Cortex, Paeoniae Radix Alba, and Cinnamomi Ramulus, peak 21 was from Moutan Cortex and Paeoniae Radix Alba, peaks 22 and 25 were from Poria, Moutan Cortex, Persicae Semen, Paeoniae Radix Alba, and Cinnamomi Ramulus, peak 26 was from Cinnamomi Ramulus, Paeoniae Radix Alba, and Persicae Semen. The similarity among the 10 batches of GFC was above 0.90. The results of validation met technical requirement of fingerprints. Sixteen chemical components were identified by UPLC-Q-TOF-MS, which were 16α-hydroxydehydrotrametenolic acid, 16α-hydroxychalcic acid, 3-oxo-6,16α-dihydroxy-lanosta-7,9(11),24(31)-trien-21-oic acid, dehydrotumulosic acid, tumulosic acid, 3-oxo-6,16α-dihydroxy-lanosta-8,24-diene-21-oic acid, eburicoic acid, polyporenic acid C, 3-epidehydrotumulosic acid, 3-O-acetyl-16α-hydroxydehydrotrametenolic acid, 3-epidehydropachymic acid, 3-O-acetyl-16α-hydroxyplugymic acid, dehydropachymic acid, pachymic acid, dehydrotrametenolic acid, and dehydroeburicoic acid. ConclusionThe method is rapid, accurate, and has desirable precision, reproducibility, and stability, which could be applied to the quality control of GFC.
引文
[1]王振中,范麒如,窦霞,等.桂枝茯苓胶囊抑制小鼠离体子宫收缩效应及其物质基础评价[J].中草药,2009,40(4):609-611.
[2]刘菊红,唐世倩,彭沙,等.桂枝茯苓胶囊联合屈螺酮炔雌醇治疗子宫内膜异位症的临床研究[J].现代药物与临床,2018,33(12):3279-3283.
[3]张华.桂枝茯苓胶囊在妇产科临床应用近况[J].中国社区医师:医学专业,2010,22(12):28-29.
[4]牛晶娟.桂枝茯苓胶囊联合孕三烯酮治疗子宫腺肌症的临床研究[J].现代药物与临床,2017,32(5):835-839.
[5]Ji X,Gao J,Cai X,et al.Immunological regulation of Chinese herb Guizhi Fuling Capsule on rat endometriosis model[J].J Ethnopharmacol,2011,134(3):624-629.
[6]Sun L,Liu L,Zong S,et al.Traditional Chinese medicine Guizhi Fuling capsule used for therapy of dysmenorrhea via attenuating uterus contraction[J].J Ethnopharmacol,2016,191:273-279.
[7]Strawn Jr E Y,Novy M J,Burry K A,et al.Insulin-like growth factor I promotes leiomyoma cell growth in vitro[J].Am J Obstet Gynecol,1995,172(6):1837.
[8]冯丽娜,洪莉.桂枝茯苓胶囊联合左炔诺孕酮宫内节育系统治疗子宫腺肌症的疗效观察[J].现代药物与临床,2017,32(8):1516-1519.
[9]中国药典[S].一部.2015.
[10]冯亚龙,赵英永,丁凡,等.茯苓皮的化学成分及药理研究进展(I)[J].中国中药杂志,2013,28(7):1098-1102.
[11]林虓,何艳梅.茯苓三萜化合物的药理作用研究进展[J].黑龙江科技信息,2014(31):77.
[12]张新庄,萧伟,徐筱杰,等.基于网络药理学的桂枝茯苓胶囊治疗痛经、子宫肌瘤和盆腔炎的分子作用机制研究[J].中草药,2016,47(1):81-94.
[13]杨鹏飞,王振中,王洪,等.桂枝茯苓胶囊化学成分研究(III)[J].中草药,2012,43(3):463-466.
[14]王振中,李成,李家春,等.桂枝茯苓胶囊化学成分研究(I)[J].中草药,2011,42(5):856-858.
[15]王洪庆,刘超,方莲花,等.桂枝茯苓胶囊化学成分研究(IV)[J].中草药,2013,44(11):1368-1390.
[16]杨鹏飞,李保明,王振中,等.HPLC法同时测定桂枝茯苓胶囊中4种茯苓三萜酸成分[J].中草药,2016,47(18):3215-3218.
[17]林夏,何艳梅,李家春,等.桂枝茯苓胶囊中三萜类成分UPLC指纹图谱研究[J].中草药,2016,47(16):2857-2862.
[18]马莹,李家春,黄文哲,等.UPLC-MS/MS同时测定桂枝茯苓胶囊中6种三萜酸类成分的含量[J].中国中药杂志,2017,42(17):3368-3373.
[2]刘菊红,唐世倩,彭沙,等.桂枝茯苓胶囊联合屈螺酮炔雌醇治疗子宫内膜异位症的临床研究[J].现代药物与临床,2018,33(12):3279-3283.
[3]张华.桂枝茯苓胶囊在妇产科临床应用近况[J].中国社区医师:医学专业,2010,22(12):28-29.
[4]牛晶娟.桂枝茯苓胶囊联合孕三烯酮治疗子宫腺肌症的临床研究[J].现代药物与临床,2017,32(5):835-839.
[5]Ji X,Gao J,Cai X,et al.Immunological regulation of Chinese herb Guizhi Fuling Capsule on rat endometriosis model[J].J Ethnopharmacol,2011,134(3):624-629.
[6]Sun L,Liu L,Zong S,et al.Traditional Chinese medicine Guizhi Fuling capsule used for therapy of dysmenorrhea via attenuating uterus contraction[J].J Ethnopharmacol,2016,191:273-279.
[7]Strawn Jr E Y,Novy M J,Burry K A,et al.Insulin-like growth factor I promotes leiomyoma cell growth in vitro[J].Am J Obstet Gynecol,1995,172(6):1837.
[8]冯丽娜,洪莉.桂枝茯苓胶囊联合左炔诺孕酮宫内节育系统治疗子宫腺肌症的疗效观察[J].现代药物与临床,2017,32(8):1516-1519.
[9]中国药典[S].一部.2015.
[10]冯亚龙,赵英永,丁凡,等.茯苓皮的化学成分及药理研究进展(I)[J].中国中药杂志,2013,28(7):1098-1102.
[11]林虓,何艳梅.茯苓三萜化合物的药理作用研究进展[J].黑龙江科技信息,2014(31):77.
[12]张新庄,萧伟,徐筱杰,等.基于网络药理学的桂枝茯苓胶囊治疗痛经、子宫肌瘤和盆腔炎的分子作用机制研究[J].中草药,2016,47(1):81-94.
[13]杨鹏飞,王振中,王洪,等.桂枝茯苓胶囊化学成分研究(III)[J].中草药,2012,43(3):463-466.
[14]王振中,李成,李家春,等.桂枝茯苓胶囊化学成分研究(I)[J].中草药,2011,42(5):856-858.
[15]王洪庆,刘超,方莲花,等.桂枝茯苓胶囊化学成分研究(IV)[J].中草药,2013,44(11):1368-1390.
[16]杨鹏飞,李保明,王振中,等.HPLC法同时测定桂枝茯苓胶囊中4种茯苓三萜酸成分[J].中草药,2016,47(18):3215-3218.
[17]林夏,何艳梅,李家春,等.桂枝茯苓胶囊中三萜类成分UPLC指纹图谱研究[J].中草药,2016,47(16):2857-2862.
[18]马莹,李家春,黄文哲,等.UPLC-MS/MS同时测定桂枝茯苓胶囊中6种三萜酸类成分的含量[J].中国中药杂志,2017,42(17):3368-3373.