Objective: To establish a method for the simultaneous determination of 28 pyrrolizidine alkaloids in honey by QuEChERS and UPLC-MS/MS, and carry out preliminary risk assessment according to the research results. Methods: The samples were prepared by QuEChERS, then separated on an ACQUITY UPLC HSS T3 column (2.1 mm×100 mm, 1.8 μm). 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 and 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 results showed that all the 28 PAs had good linearity in 1-20 ng·mL-1 with the correlation coefficients higher than 0.99. The average recoveries of all the 28 PAs were between 71.8% and 103.5%, with the RSDs of 3.3%-9.2%. The limits of quantifications (LOQs) of 28 PAs were between 0.20 ng·mL-1 and 0.90 ng·mL-1. PAs was detected in 10 of 30 samples, and the total contents of positive samples were 4.85-78.34 μg·kg-1. Conclusion: The established method can simultaneously determine 28 pyrrolizidine alkaloids in honey. The preliminary risk assessment shows that there is a certain risk of drug safety.
ZAN Ke, LI Yao-lei, WANG Ying, LIU Li-na, JIN Hong-yu, ZUO Tian-tian, MA Shuang-cheng
. Risk assessment and fast determination of 28 pyrrolizidine alkaloids in honey by QuEChERS method and UPLC-MS/MS*[J]. Chinese Journal of Pharmaceutical Analysis, 2021
, 41(12)
: 2087
-2094
.
DOI: 10.16155/j.0254-1793.2021.12.06
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