白背三七中吡咯里西啶生物碱的含量分析及风险评价

Content analysis and risk assessment of pyrrolizidine alkaloids in Gynura divaricata(L.)DC.

目的建立超高效液相色谱串联质谱法(ultra performance liquid chromatograph tandem mass spectrometry,UPLC-MS/MS)测定白背三七中芝麻菜叶千里光碱-N-氧化物、春千里光碱、野百合碱、春千里光碱-N-氧化物、倒千里光碱、千里光菲灵碱和千里光宁碱的含量,依据检测结果对其进行初步风险评价。方法用Agilent Poroshell 120 SB-C_(18)色谱柱(150 mm×3.0 mm,2.7μm),流动相A为1 mL·L^(-1)甲酸和5.0 mmol·L^(-1)甲酸铵水溶液,B为1 mL·L^(-1)甲酸的甲醇,梯度洗脱。电喷雾离子源,正离子多反应模式监测。结果7种吡咯里西啶生物碱在各自质量浓度范围内线性关系良好(r>0.9970);平均加样回收率为89.31%~92.16%,RSD值为2.02%~3.48%。5批白背三七样品中倒千里光碱的含量范围为158.76~1714.89μg·kg^(-1)。结论建立的UPLC-MS/MS法稳定可行,可为白背三七中吡咯里西啶生物碱的质量控制和安全性评价提供科学依据。

Objective To establish a method for the simultaneous determination of erucifoline N-oxide,senecivernine,crotaline,senecivernine N-oxide,retrorsine,seneciphylline and senecionine in Gynura divaricata(L.)DC.by ultra performance liquid chromatograph tandem mass spectrometry(UPLC-MS/MS),and to carry out risk assessment according to the research results.Methods The assay was performed on an Agilent Poroshell 120 SB-C_(18) column(150 mm×3.0 mm,2.7μm)and the sample was eluted with a gradient mobile phase consisting of 1 mL·L^(-1) formic acid and 5.0 mmol·L^(-1) ammonium formate in water-1 mL·L^(-1) formic acid in methanol.The MS system was operated by using electrospray ionization in the positive ion mode,and the scan mode was in multiple reactions monitoring mode.Results Seven pyrrolizidine alkaloids showed good linear relationships within their own ranges(r>0.9970).The average recoveries were 89.31%-92.16%with RSD of 2.02%-3.48%.The content ranges of retrorsine in the 5 batches of Gynura divaricata(L.)DC.were 158.76-1714.89μg·kg^(-1).Conclusion The method established in this study provides a scientific basis for the quality control and safety evaluation of pyrrolizidine alkaloids in Gynura divaricata(L.)DC.