基于UPLC-Q-TOF-MS法砂烫马钱子化学成分定性研究
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摘要
目的应用超高效液相色谱-四级杆串联飞行时间质谱法(UPLC-Q-TOF-MS)对砂烫马钱子提取物的主要化学成分进行定性研究。方法采用Agilent SB-C_(18)(2.1 mm×100 mm,1.8μm)色谱柱,以0.1%甲酸水(A)-乙腈(B)溶液为流动相,梯度洗脱,流速为0.2 mL·min~(-1),柱温为35°C;质谱分析采用信息关联模式(IDA)正、负离子分别采集。结果共鉴定出砂烫马钱子提取物中24个化学成分,其中有8个为马钱子文献中首次报道,并在负离子模式下发现3个新化合物;主要成分包括生物碱、脂肪酸酯、糖苷、甾醇等。结论该方法精确、可靠、高效,适用于砂烫马钱子成分的快速鉴定,能为马钱子炮制品的开发利用以及阐明其药效物质基础提供参考。
Objective To analyse and identify main chemical constituents in extract of sand stir-baked Strychni Semen by UPLC-Q-TOF-MS. Methods Using Agilent SB-C18(2.1 mm×100 mm,1.8 μm) column with gradient elution consisting of 0.1 % formic acid in water(A) and acetonitrile(B),at a flow rate of 0.2 mL?min~(-1). The column temperature was set at 35 ℃. MS analysis was based on information associated mode(IDA) that positive and negative ions were collected seperately. Results We identified a total of 24 compounds in sand stir-baked Strychni Semen,of which 8 have not been reported as from Strychni Semen,3 new compounds were found in the negative ion mode. The main chemical constituents include alkaloids,fatty acid esters,glycosides,sterols,etc.Conclusion The method established is accurate,reliable,and efficient,and is suitable for rapid identification of ingredients in sand stir-baked Strychni Semen. It provides a reference for the development and utilization of processed products of Strychni Semen and clarify its efficacy and material basis.
Objective To analyse and identify main chemical constituents in extract of sand stir-baked Strychni Semen by UPLC-Q-TOF-MS. Methods Using Agilent SB-C18(2.1 mm×100 mm,1.8 μm) column with gradient elution consisting of 0.1 % formic acid in water(A) and acetonitrile(B),at a flow rate of 0.2 mL?min~(-1). The column temperature was set at 35 ℃. MS analysis was based on information associated mode(IDA) that positive and negative ions were collected seperately. Results We identified a total of 24 compounds in sand stir-baked Strychni Semen,of which 8 have not been reported as from Strychni Semen,3 new compounds were found in the negative ion mode. The main chemical constituents include alkaloids,fatty acid esters,glycosides,sterols,etc.Conclusion The method established is accurate,reliable,and efficient,and is suitable for rapid identification of ingredients in sand stir-baked Strychni Semen. It provides a reference for the development and utilization of processed products of Strychni Semen and clarify its efficacy and material basis.
引文
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[16]马密霞,胡文祥,刘接卿,等.马钱子属植物的药理毒理作用及临床应用进展[J].中国医院药学杂志,2007,27(12):1725-1728.
[2]赵引利,何燕宁,杨宇杰,等.马钱子及其制剂药动学研究进展[J].中草药,2015,46(11):1710-1714.
[3]林昌松,陈纪藩,刘晓玲,等.马钱子药理研究及临床应用概况[J].中药新药与临床药理,2006,17(2):158-161.
[4]刘玉杰,吴伯英,徐颖,等.马钱子本草考证与炮制沿革研究[J].中药与临床,2014,5(2):90-92.
[5]JIANG Y H,YANG W L,GONG Q F.HPLC determination of strychnine and brucine in semen strychni and its processed products[J].China Journal of Chinese Materia Medica,2002,27(12):899-901.
[6]徐颖,刘玉杰,孙涛,等.砂烫马钱子炮制工艺优选[J].中国实验方剂学杂志,2013,19(5):25-28.
[7]汤淮波,吴萍,胡海,等.改良砂烫法炮制马钱子的实验研究[J].中南药学,2010,8(6):461-464.
[8]国家药典委员会.中华人民共和国药典:一部[M].北京:中国医药科技出版社,2015:313.
[9]ZOU J G,XU X L,LIU Y Y,et al.Ultrasonic-assisted extraction of alkaloids from semen strychni by response surface analysis[J].Food Science,2009,30(16):111-114.
[10]CHEN J,HOU T,FANG Y,et al.HPLC determination of strychnine and brucine in rat tissues and the distribution study of processed semen strychni[J].Yakugaku Zasshi:Journal of the Pharmaceutical Society of Japan,2011,131(5):721-729.
[11]解宝仙,唐文照,王利红,等.马钱子化学成分研究[J].中药材,2016,39(1):86-89.
[12]解宝仙,唐文照,王晓静.马钱子的化学成分和药理作用研究进展[J].药学研究,2014,33(10):603-606.
[13]刘艳萍.马钱子的化学成分研究[D].济南:山东大学,2010.
[14]刘锡葵,李薇.马钱子果化学成分研究[J].中草药,1998,29(7):435-438.
[15]过振华,马红梅,张伯礼.马钱子药理毒理研究回顾及安全性研究展望[J].中国药物警戒,2012,9(1):645-649.
[16]马密霞,胡文祥,刘接卿,等.马钱子属植物的药理毒理作用及临床应用进展[J].中国医院药学杂志,2007,27(12):1725-1728.