QTRAP-UPLC-MS/MS同时测定玄参不同产地及商品药材中10种核苷类成分的含量
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摘要
目的:建立超高效液相色谱-三重四级杆/线性离子阱质谱(QTRAP-UPLC-MS/MS)同时测定玄参不同产地及商品药材中10种核苷类成分的方法。方法:采用Waters Atlantis T3C18色谱柱(2.1 mm×150mm,3μm),以甲醇-5 mmol·L-1醋酸铵(含0.1%冰醋酸)为流动相,0.4 m L·min-1梯度洗脱,正离子多反应监测(MRM)模式测定。结果:10种核苷类成分的浓度与峰面积的线性关系良好(r2>0.994 7);平均加样回收率为94.72%~98.18%。玄参核苷类成分中,以鸟苷、尿苷、腺苷、尿嘧啶含量较高;不同产地及商品药材中核苷类成分含量有所差异。结论:该方法准确、可靠,为玄参药材内在质量的综合评价提供新的方法参考。
Objective: To establish a QTRAP-UPLC-MS /MS method for simultaneous determination of 10 kinds of nucleosides and nucleobases in Scrophulariae Radix from different habitats and commercial herbs. Methods: The analysis was carried out on an Waters Atlantis T3C18column( 2. 1 mm × 150 mm,3 μm) which was eluted by a mobile phase of methanol-5 mmol·L- 1ammonium acetate( 0. 1% acetic acid) at a flow rate of 0. 4 m L·min- 1. The target compounds were analyzed by the positive ion multiple reaction monitoring( MRM) mode. Results: Ten kinds of nucleosides and nucleobases showed a good linearity( r2> 0. 994 7) in the range of the tested concentrations. The average recoveries of the ten components were between 94. 72% and 98. 18%. The contents of guanosine,uridine,adenosine and uracil were higher in Scrophulariae Radix. The contents were different from different habitats and commercial herbs. Conclusion: The established method is accurate and reliable,and provides a scientific basis for the quality evaluation of Scrophulariae Radix.
Objective: To establish a QTRAP-UPLC-MS /MS method for simultaneous determination of 10 kinds of nucleosides and nucleobases in Scrophulariae Radix from different habitats and commercial herbs. Methods: The analysis was carried out on an Waters Atlantis T3C18column( 2. 1 mm × 150 mm,3 μm) which was eluted by a mobile phase of methanol-5 mmol·L- 1ammonium acetate( 0. 1% acetic acid) at a flow rate of 0. 4 m L·min- 1. The target compounds were analyzed by the positive ion multiple reaction monitoring( MRM) mode. Results: Ten kinds of nucleosides and nucleobases showed a good linearity( r2> 0. 994 7) in the range of the tested concentrations. The average recoveries of the ten components were between 94. 72% and 98. 18%. The contents of guanosine,uridine,adenosine and uracil were higher in Scrophulariae Radix. The contents were different from different habitats and commercial herbs. Conclusion: The established method is accurate and reliable,and provides a scientific basis for the quality evaluation of Scrophulariae Radix.
引文
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[14]钟倩霞,吕广萍,彭亮,等.高效液相色谱法测定不同产地棘托竹荪中4个核苷含量[J],药物分析杂志,2014,34(3):411-414.
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[18]张婷婷,曾明飞,金燕,等.反相高效液相色谱-串联质谱法测定母乳及奶粉中核苷和核苷酸的含量[J].分析化学,2014,42(4):585-591.
[19]LI F,DUAN JA,QIAN D,et al.Comparative analysis of nucleosides and nucleobases from different sections of Elaphuri Davidiani Cornu and Cervi Cornu by UHPLC-MS/MS[J].J Pharm Biomed Anal,2013,83:10-18.
[20]YI LP,PING X,XIANG L,et al.Determination of nucleosides and nucleobases in Isatidis Radix by HILIC-UPLC-MS/MS[J].Ana Methods,2013,5(22):6395-6400.
[21]再帕尔·阿不力孜,李斌,阿布拉江·克依木,等.新型QTRAPTM四极杆-线性离子阱串联质谱仪的特点及应用[J].现代仪器,2004,10(5):9-13.
[2]胡瑛瑛,黄真.玄参的化学成分及药理作用研究进展[J].浙江中医药大学学报,2008,32(2):268-270.
[3]韩建军,宁娜.玄参药理作用的研究概述[J].海峡药学,2014,26(12):97-99.
[4]严宜昌,张丽萍,黄鹤,等.恩施玄参GAP生产基地的产地适应性分析[J].亚太传统医药,2009,5(9):57-59.
[5]邢振杰.中药材种植业的演变与发展[J].中国现代中药,2011,13(5):53-55.
[6]徐绍清,徐永江,金水虎,等.浙江省玄参科归化新记录——凯氏草属[J].防护林科技,2015,1:50-51.
[7]王明军.中药“浙八味”道地性的科学性品质及其文化研究初探[J].中药材,2007,30(5):505-508.
[8]李杰,詹垮垮,段时振,等.中药玄参研究概况[J].湖北中医杂志,2013,35(8):73-75.
[9]吕爱娟,吴皓.中药中核苷类成分的研究进展[J].中国中医药信息杂志,2006,7(13):94-97.
[10]张雪梅,王瑞,安睿,等.HPLC同时测定玄参中5种成分的含量[J].中国中药杂志,2011,36(6):709-711.
[11]张雪梅,王瑞,吴喜民,等.优化分光光度法用于玄参中总环烯醚萜类成分的含量测定[J].中成药,2011,33(2):308-311.
[12]王建华,谢丽华,刘洪宇,等.玄参不同加工品中哈巴俄苷与肉桂酸的HPLC含量测定[J].中国药学杂志,2000,35(6):15-18.
[13]肖珊珊,金郁,郭怀忠,等.RP-HPLC法测定板蓝根药材中核昔类成分的含量[J].药物分析杂志,2006,26(1):48-50.
[14]钟倩霞,吕广萍,彭亮,等.高效液相色谱法测定不同产地棘托竹荪中4个核苷含量[J],药物分析杂志,2014,34(3):411-414.
[15]ZHANG WM,FU WW,SUN MY,et al.Simultaneous determination of five nucleosides and nucleobases of Rehmannia glutinosa Libosch.by high performance liquid chromatography[J].Acta Pharmaceutica Sinica,2011,46(11):1380-1384.
[16]JAMES IL,TOM DM,SALAH E,et al.Rapid Commum[J].Mass Sp,1993,7:427-434.
[17]杨丰庆,张雪梅,葛莉亚,等.毛细管电泳-质谱联用法测定灵芝药材中核苷类成分[J].中国药科大学学报,2011,42(4):337-341.
[18]张婷婷,曾明飞,金燕,等.反相高效液相色谱-串联质谱法测定母乳及奶粉中核苷和核苷酸的含量[J].分析化学,2014,42(4):585-591.
[19]LI F,DUAN JA,QIAN D,et al.Comparative analysis of nucleosides and nucleobases from different sections of Elaphuri Davidiani Cornu and Cervi Cornu by UHPLC-MS/MS[J].J Pharm Biomed Anal,2013,83:10-18.
[20]YI LP,PING X,XIANG L,et al.Determination of nucleosides and nucleobases in Isatidis Radix by HILIC-UPLC-MS/MS[J].Ana Methods,2013,5(22):6395-6400.
[21]再帕尔·阿不力孜,李斌,阿布拉江·克依木,等.新型QTRAPTM四极杆-线性离子阱串联质谱仪的特点及应用[J].现代仪器,2004,10(5):9-13.