作　　者： ; ;

机构地区： 广州中医药大学第二临床医学院

出　　处： 《中国实验方剂学杂志》 2019年第17期152-159,共8页

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,1.7μm);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m/z 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 2~18.24μg·L-1线性关系良好(r≥0.994 8),平均加样回收率为93.73%~104.34%,RSD均<5%(n=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。 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,1.7μm)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 m/z 142.10/44.11 for arecaine,m/z 156.20/44.07 for arecoline,m/z 314.29/265.12 for norisoboldine and m/z 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 2-18.24μg·L-1,respectively.The average recoveries of the above compounds ranged from 93.73%to 104.34%,with RSD(n=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： 香槟方 生物碱 超高效液相色谱 串联质谱法 槟榔次碱 槟榔碱 去甲异波尔定 波尔定碱

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