Abstract
A simple and high sensitive ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed and validated for the simultaneous determination of peimine and peiminine in beagle dog plasma after the oral administration of Fritillariae ussuriensis Maxim and Fritillariae thunbergii Miq powder. Chromatographic separation was achieved on an ACQUIT UPLC® BEH C18 column (1.7 μm, 2.1 × 100 mm) in a gradient elution way with a mobile phase consisting of acetonitrile and water containing 0.1% formic acid at a flow rate of 0.4 mL/min. The plasma samples were prepared by a liquid–liquid extraction (LLE) method with ethyl acetate. The analytes were detected with a triple quadrupole tandem mass spectrometry (MS) in multiple reaction monitoring (MRM) mode and a positive ion electrospray ionization (ESI) of the transitions at m/z 432.4→414.4 for peimine and m/z 430.3→412.3 for peiminine. The method was linear for two analytes over the investigated range with all determined correlation coefficients exceeding 0.9900. The lower limit of quantification (LLOQ) was 0.988 ng/mL for peimine and 0.980 ng/mL for peiminine. The mean extraction recoveries of peimine and peiminine at three quality control samples (QC) levels were ranged from 82.56 to 88.71%, and matrix effects ranged from 92.06 to 101.2%. The intra-day and inter-day precision and accuracy were within the acceptable limits at LLOQ and QC levels. The method was effectively and successfully applied to the pharmacokinetics of peimine and peiminine after oral administration of powder to beagle dogs. The obtained results may be help to guide the clinical application of Fritillaria ussuriensis Maxim and Fritillaria thunbergii Miq.
Highlights
Bulbus fritillaria is recorded with the Chinese name “Bei Mu” in classical Chinese medicine books, and has been used as a traditional medicine for thousands of years [1]
We developed a rapid, high-sensitivity, high-performance liquid chromatography–mass spectrometry (UPLC-MS/MS) combined multiple reaction monitoring (MRM) technique for the simultaneous determination of peimine and peiminine in beagle dog plasma for the first time
The results showed that a mobile phase of acetonitrile–water exhibited satisfactory peak shape and sensitivity
Summary
Bulbus fritillaria is recorded with the Chinese name “Bei Mu” in classical Chinese medicine books, and has been used as a traditional medicine for thousands of years [1]. Bulbus fritillaria is the dried bulbus of Fritillaria ussuriensis Maxim (FU) or Fritillaria thunbergii Miq (FT) in the genus Fritillaria Liliaceae family) [2,3]. FU, known as “Ping-beimu,” is recorded officially, and it has been previously reported that a number of alkaloids are major biologically active components [4]. FT is often referred to as “Zhe-beimu” [5]. This plant is mainly grown in the Heilongjiang, Zhejiang ,and Jiangsu provinces of China. Peimine and peiminine are selected as the phytochemical marker compounds of FU and FT for quality control according to the 2015 edition of The Pharmacopoeia of the People’s Republic of Molecules 2018, 23, 1573; doi:10.3390/molecules23071573 www.mdpi.com/journal/molecules
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