Objective： To establish a method for the simultaneous determination of six main pyrrolizidine alkaloids （lycopsamine,rinderine,echinatine,rinderine N-oxide,echinatine N -oxide,and lycopsamine N -oxide） in Agerati Conyzoidis Herba by UPLC-MS/MS. And to carry out preliminary risk assessment according to the research results. Methods： The assay was performed on a ACQUITY UPLC HSS T3 column（ 2.1 mm×100 mm,1.8 μm） and the sample was eluted with a gradient mobile phase consisting of 0.05% formic acid and 2.5 mmol·L-1 ammonium formate in water（A）-0.05% formic acid and 2.5 mmol·L-1 ammonium formate in acetonitrile（B）,the flow rate was 0.3 mL·min-1,the column temperature was 40 ℃. The MS system was operated by using electrospray ionization（ESI） in the positive ion mode,and the scan mode was in multiple reactions monitoring（MRM） mode. External standard method was used in the experiment. Results： The linear ranges of lycopsamine,rinderine,echinatine,rinderine N-oxide,echinatine N -oxide,and lycopsamine N -oxide were 0.972-97.2,0.964-96.4,1.016-101.6,1.056-105.6,1.032-103.2 and 0.958-95.8 ng·mL-1,respectively（r> 0.999 0）. The average recoveries were 88.5%,90.2%,92.6%,94.3%,91.8% and 95.7% with RSD of 3.1%,3.5%, 2.4%,2.1%,2.5% and 3.2%,respectively. The content ranges of lycopsamine,rinderine,echinatine,rinderine N-oxide,echinatine N-oxide,and lycopsamine N-oxide in the 6 batches of Agerati Conyzoidis Herba were 1.22- 2.87,0.36-0.75,4.23-10.65,1.08-3.65,10.31-24.26 and 5.25-13.36 μg·g-1,respectively. Conclusion： The established method can simultaneously determine six pyrrolizidine alkaloids in Agerati Conyzoidis Herba. The preliminary risk assessment showes that there is a certain risk of drug safety.
ZAN Ke, LI Yao-lei, WANG Ying, WANG Zhao, JIN Hong-yu, LIU Li-na, MA Shuang-cheng
. Risk assessment and determination of six main pyrrolizidine alkaloids in Agerati Conyzoidis Herba by UPLC-MS/MS*[J]. Chinese Journal of Pharmaceutical Analysis, 2021
, 41(7)
: 1169
-1175
.
DOI: 10.16155/j.0254-1793.2021.07.08
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