Quality assessment of Dandeng Tongnao Soft Capsule based on UPLC- Q-Orbitrap HRMS combined with principal component analysis / 中草药

ABSTRACT

Objective To establish a quantitative analysis method of multiple active components in Dandeng Tongnao Soft Capsule (DTSC) based on ultra performance liquid chromatography-quadrupole/orbitrap high resolution mass spectrometry (UPLC-Q-Orbitrap HRMS), and conduct a quality assessment using principal component analysis. Methods The column was Acquity UPLC® BEH C18 (50 mm × 2.1 mm, 1.7 μm) and the mobile phase was consisted of acetonitrile-water (containing 0.1% formic acid) with gradient elution; the information of accurate mass and fragment ions was obtained by the novel “monitored simultaneously for positive and negative ions, full MS scan and automatic trigger secondary mass spectrometry” mode of Q-Orbitrap MS technology to ensure the accurate qualitation and quantitation of the analytes; the results of the contents were then combined with the principal component analysis to achieve the scientific assessment of the different batches of drugs. Results Under the optimized conditions, betaine, danshensu, chlorogenic acid, protocatechuic aldehyde, puerarin, caffeic acid, galuteolin, rosmarinic acid, salvianolic acid A, salvianolic acid B, quercetin, apigenin, senkyunolide A, dihydrotanshinone I, tanshinone I, cryptotanshinone, and tanshinon IIA all showed good liner relationship (r ≥ 0.999 2) in the range of 0.018 1-0.578 4, 5.555 7-177.782 0, 0.018 1-0.580 3, 0.002 8-0.089 2, 0.787 2-25.191 3, 0.000 5-0.016 7, 0.007 2-0.228 9, 0.065 8-2.105 3, 0.304 6-9.747 1, 3.888 1-124.417 6, 0.000 5-0.016 0, 0.000 6-0.018 1, 0.002 5-0.080 1, 0.019 8-0.632 8, 0.032 2-1.031 7, 0.102 8-3.290 0, and 0.044 5- 1.422 9 μg/mL, respectively; The results of the accuracy, repeatability, and stability all reached the standards (RSD ≤ 5%); The recoveries ranged from 98% to 102% and RSDs were below 3%; The analysis results showed that the quality of the most batches was stable, tanshinone I, cryptotanshinone, dihydrotanshinone I, and tanshinon IIA had a great influence on the quality of the drug, which could be monitored to ensure the quality of different batches. Conclusion The methods established in this paper have a high sensitivity and accuracy; the results of the methodology conform to the relevant requirements and the methods can rapidly determinate the multiple active components in DTSC; The research also provides a new scientific basis and reference for the quality assessment at the same time.