高效液相色谱-串联质谱法快速检测植物药酒中的40种生物碱

目的 建立高效液相色谱-串联三重四极杆质谱(high performance liquid chromatography-tandem triple quadrupole mass spectrometry,HPLC-MS/MS)法快速检测植物药酒中40种生物碱的分析方法.方法 样品采用乙腈提取,提取液经N-丙基乙二胺...

Rapid determination of 40 kinds of alkaloids in botanical medicated wines by high performance liquid chromatography-tandem mass spectrometry

Objective To establish a analysis method for the rapid determination of 40 kinds of alkaloids in botanical medicated wine by high performance liquid chromatography-tandem triple quadrupole mass spectrometry(HPLC-MS/MS). Methods The sample was extracted by acetonitrile, purified by N-propyl ethylenediamine adsorbent,condensed by nitrogen blowing. The residues were redissolved with the initial mobile phase solution. The solution was separated with a Waters CORTECS C₁₈+ column(100 mm×3.0 mm, 2.7 μm) using acetonitrile-5 mmol/L ammonium formate(containing 0.1% formic acid) aqueous solution as mobile phase for gradient elution. Mass spectrometry with electrospray ionization in positive mode and multiple reaction monitoring were used for alkaloids qualitative and quantitative analysis. Results All the 40 kinds of alkaloids had good linear relationship, the limits of detection were 0.03-0.30 μg/L, and the limits of quantification were 0.1-1.0 μg/L. The 3 level standard addition recovery test of low,medium and high concentration was carried out on the botanical wine, and the recoveries were 60.1%-100.5%, and the relative standard deviations were 1.8%-14.4%(n=6). Conclusion The method has the advantages of fast and simple sample pretreatment, high detection sensitivity and good selectivity, and is suitable for the rapid analysis of various alkaloids in large quantities of botanical medicated wine samples.