Objective: To establish an ultra-performance liquid chromatography-triple quadrupole tandem mass spectrometry (UPLC-QQQ MS/MS) method for the determination of genotoxic lucidin and lucidin-3-O-primeveroside in raw and processed Rubiae Radix et Rhizoma. Methods: The analysis was performed on a Waters ACQUITY UPLC BEH C18 column (100 mm×2.1 mm, 1.7 μm) using 0.1% formic acid-acetonitrile as the mobile phase in gradient elution mode. The flow rate was set at 0.3 mL · min-1, the column temperature was maintained at 30 ℃, and the injection volume was 1 μL. Detection was carried out by mass spectrometry with ESI+ ionization mode and multiple reaction monitoring (MRM). Additionally, the results from different grades of medicinal materials were analyzed using cluster analysis and partial least squares-discriminant analysis (PLS-DA) models. Results: Lucidin and lucidin 3-O-beta-primveroside were found to exhibit good linearity (r>0.990 0) within their respective concentration ranges. The mean recovery rates were determined to be 99.8% and 98.3% with RSDs of 1.1% and 1.2%, respectively. Content of lucidin in the prepared slices were 6.51-26.28 μg · g-1, while those of lucidin-3-O-primeveroside were 85.77-232.73 μg · g-1. Contents of lucidin and lucidin-3-O-primeveroside in the incompletely processed Rubiae Radix et Rhizoma charcoal were 5.13-12.45 μg · g-1, 33.31-196.52 μg · g-1.In properly processed Rubiae Radix et Rhizoma charcoal, content of lucidin were 15.78-40.85 μg · g-1, whereas those of lucidin-3-O-primeveroside was reduced to undetectable or trace levels (0-16.12 μg · g-1). Conclusion: This study establishes a reliable method for quantifying lucidin and lucidin-3-O-primeveroside in Rubiae Radix et Rhizoma. The method demonstrates excellent accuracy, stability, reproducibility, and robustness, making it suitable for routine content analysis. The charcoal-processing (stir-frying) procedure significantly alters the content levels of these genotoxic substances.
JIANG Kai-hang
,
ZHANG Ming-tong
,
LI Zhi-bing
,
FENG Xue-ying
,
LIU Zhi-hao
,
LI Zi-bin
,
LIU Dong-sheng
,
LI Dong-hua
,
MA Xiao
. Determination of genotoxic lucidin and lucidin 3-O-beta-primveroside in raw and processed Rubiae Radix et Rhizoma based on UPLC-QQQ MS/MS*[J]. Chinese Journal of Pharmaceutical Analysis, 2025
, 45(4)
: 679
-685
.
DOI: 10.16155/j.0254-1793.2024-1089
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