Simultaneous Determination of Four Alkaloid Components in Xiangbin Decoction by UPLC-QqQ-MS/MS

Si-wei JIANG; Zuo-liang ZHENG; Fang-fang XU; Wei-ying CHEN; Li-peng TANG; Zhi-qiang CHEN; Bo LIU; Ben LI

doi:10.13422/j.cnki.syfjx.20191718

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Simultaneous Determination of Four Alkaloid Components in Xiangbin Decoction by UPLC-QqQ-MS/MS

Resource and Quality Evaluation | 更新时间：2021-02-09

- Simultaneous Determination of Four Alkaloid Components in Xiangbin Decoction by UPLC-QqQ-MS/MS
- Chinese Journal of Experimental Traditional Medical Formulae Vol. 25, Issue 17, Pages: 152-159(2019)
- 作者机构：
  
  1.广州中医药大学　第二临床医学院，广州　 510006；
  2.广州中医药大学　广东省中医证候临床研究重点实验室，广州　 510006
- 作者简介：
- 基金信息：
- DOI：10.13422/j.cnki.syfjx.20191718
  CLC： R284.2; R285; R22; R2-031
- Received：27 March 2019，
  
  Published Online：21 May 2019，
  
  Published：05 September 2019
- 稿件说明：
移动端阅览
Si-wei JIANG, Zuo-liang ZHENG, Fang-fang XU, et al. Simultaneous Determination of Four Alkaloid Components in Xiangbin Decoction by UPLC-QqQ-MS/MS[J]. Chinese journal of experimental traditional medical formulae, 2019, 25(17): 152-159.
DOI：

Si-wei JIANG, Zuo-liang ZHENG, Fang-fang XU, et al. Simultaneous Determination of Four Alkaloid Components in Xiangbin Decoction by UPLC-QqQ-MS/MS[J]. Chinese journal of experimental traditional medical formulae, 2019, 25(17): 152-159. DOI： 10.13422/j.cnki.syfjx.20191718.

摘要

目的：

建立超高效液相色谱-三重四极杆质谱法(UPLC-QqQ-MS/MS)同时测定香槟方中槟榔次碱、槟榔碱、去甲异波尔定、波尔定碱的含量，比较槟榔、乌药单煎液与香槟方合煎液中4种生物碱成分的含量变化，为香槟方制剂研究提供实验基础。

方法：

采用Waters ACQUITY UPLC BEH Shield RP18色谱柱(2.1 mm×150 mm，1.7 μm)；流动相0.1%甲酸水溶液-乙腈梯度洗脱，流速0.2 mL·min

－1

，柱温30 ℃；采用电喷雾离子源(ESI)，正离子模式扫描，多反应监测(MRM)模式检测；各化合物的定量离子对分别为

142.10/44.11(槟榔次碱)，156.20/44.07(槟榔碱)，314.29/265.12(去甲异波尔定)，328.13/265.10(波尔定碱)。

结果：

槟榔次碱、槟榔碱、去甲异波尔定、波尔定碱分别在0.479 0～57.48，0.976 0～78.08，0.812 0～64.96，0.091 2～18.24 μg·L

－1

线性关系良好(

≥0.994 8)，平均加样回收率为93.73%～104.34%，RSD均

5%(

＝6)。香槟方中槟榔次碱、槟榔碱、去甲异波尔定、波尔定碱的质量分数分别为(90.07±1.26)，(445.27±12.39)，(742.35±38.39)，(38.50±3.33)μg·g

－1

，均显著低于单煎液中的含量。

结论：

该方法快速、灵敏、准确、重复性好，可用于香槟方中生物碱成分的含量测定，为香槟方的质量控制及深入研究提供参考依据；香槟方配伍对槟榔次碱、槟榔碱、去甲异波尔定、波尔定碱的溶出量具有显著影响。

Abstract

Objective:

To establish a quantitative method for the simultaneous determination of arecaine

arecoline

norisoboldine and boldine in Xiangbin decoction by ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-QqQ-MS/MS)

and compare the variation of their contents between single and mixed decoctions.

Method:

The separation was carried on a Waters ACQUITY UPLC BEH Shield RP18(2.1 mm×150 mm

1.7 μm)column

with 0.1%formic acid solution-acetonitrile as mobile phase for gradient elution. The flow rate was 0.2 mL·min

-1

and the column temperature was 30 ℃. The quantitative MRM transitions of the four components were

142.10/44.11 for arecaine

156.20/44.07 for arecoline

314.29/265.12 for norisoboldine and

328.13/265.10 for boldine. The determination was performed in multiple reaction monitoring (MRM) mode by mass spectrometry with electrospray ionization (ESI) source under positive mode.

Result:

The linear ranges of arecaine

arecoline

norisoboldine and boldine were 0.479 0-57.48

0.976 0-78.08

0.812 0-64.96

0.091 2-18.24 μg·L

-1

respectively. The average recoveries of the above compounds ranged from 93.73%to 104.34%

with RSD (

=6) of less than 5%. The contents of arecoline

arecoline

norbibeldine and boltinine in Xiangbin decoction were (90.07±1.26)

(445.27±12.39)

(742.35±38.39)

(38.50±3.33) μg·g

-1

which were significantly lower than the contents in Linderae Radix and Arecae Semen.

Conclusion:

The method is rapid

sensitive

accurate and reproducible

and suitable for the simultaneous determination of multiple components in Xiangbin decoction

so as to provide a basis for the quality control of Xiangbin decoction. The compatibility of Xiangbin decoction has a significant effect on the dissolution contents of arecaine

arecoline

norisoboldine and boldine.

关键词

Keywords

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