Journal of Pharmaceutical Analysis ( IF 8.8 ) Pub Date : 2022-01-26 , DOI: 10.1016/j.jpha.2022.01.001 Xuan Yu 1, 2 , Wei Niu 1 , Ya-Ya Wang 1, 3 , Olajide E Olaleye 1 , Jia-Nan Wang 1, 2 , Meng-Yuan Duan 1, 2 , Jun-Ling Yang 1 , Rong-Rong He 1 , Zi-Xuan Chu 1, 2 , Kai Dong 4 , Gui-Ping Zhang 4 , Chang-Xiao Liu 5 , Chen Cheng 1 , Chuan Li 1, 2, 3
XueBiJing is an intravenous five-herb injection used to treat sepsis in China. The study aimed to develop a liquid chromatography-tandem mass spectrometry (LC-MS/MS)- or liquid chromatography-ultraviolet (LC-UV)-based assay for quality evaluation of XueBiJing. Assay development involved identifying marker constituents to make the assay therapeutically relevant and building a reliable one-point calibrator for monitoring the various analytes in parallel. Nine marker constituents from the five herbs were selected based on XueBiJing's chemical composition, pharmacokinetics, and pharmacodynamics. A selectivity test (for “similarity of response”) was developed to identify and minimize interference by non-target constituents. Then, an intercept test was developed to fulfill “linearity through zero” for each analyte (absolute ratio of intercept to C response, <2%). Using the newly developed assays, we analyzed samples from 33 batches of XueBiJing, manufactured over three years, and found small batch-to-batch variability in contents of the marker constituents (4.1%–14.8%), except for senkyunolide I (26.5%).