Abstract: This study aimed to quantitatively evaluate the contents and in vivo exposure levels of 11 primary components in six commercially available Angong Niuhuang Pill (ANP) products. A chromatography-tandem mass spectrometry (LC-MS/MS) method was developed for the simultaneous quantification of deoxycholic acid (DCA), cholic acid (CA), hyodeoxycholic acid (HDCA), glycocholic acid (GCA), taurocholic acid (TCA), curcumin (CC), baicalin (BC), berberine (BBR), and crocetin (CRT). A gas chromatography-mass spectrometry (GC-MS) method was established to determine muscone (MCN) and borneol (BN). The analytical methods were validated and applied to assess the content of the 11 components in six ANP products and their plasma exposure levels following intragastric administration in rats (All animal experiments had been approved by the Experimental Animal Ethics Committee of China Pharmaceutical University, ethics number: 2024-07-131). The quantitative methods utilizing LC-MS/MS and GC-MS were successfully established and validated for the simultaneous quantification of DCA, CA, HDCA, GCA, TCA, CC, BC, BBR, CRT, MCN and BN both in vivo and in vitro samples, respectively. The contents of HDCA, DCA, CA, GCA, TCA, CC, BC, CRT, BBR, BN and MCN varied over the ranges between 0.22 ± 0.03-1.47 ± 0.41, 0.22 ± 0.03-1.48 ± 0.39, 0.65 ± 0.01-4.28 ± 0.30, 0.44 ± 0.01-0.80 ± 0.02, 0.49 ± 0.05-1.36 ± 0.04, 0.001 2 ± 0.000 1-0.007 1 ± 0.001 0, 3.49 ± 0.80-4.47 ± 0.13, 0.003 6 ± 0.001 1-0.013 7 ± 0.014 8, 1.77 ± 0.05-4.84 ± 0.41, 4.70 ± 2.09-10.91 ± 3.08, 0.20 ± 0.03-0.44 ± 0.04 mg·g^-1, respectively. Similarly, the in vivo plasma exposure of HDCA, DCA, CA, GCA, TCA, BC, CRT covered the ranges over 5 088.63 ± 2 701.16-11 819.10 ± 7 585.61, 3 639.42 ± 1 970.63-18 853.46 ± 18 309.75, 19 397.89 ± 9 464.21-182 870.72 ± 236 816.06, 11 011.97 ± 4 236.99-57 331.79 ± 76 180.09, 53 607.57 ± 43 279.12-109 961.78 ± 82 288.37, 590.17 ± 175.72-2 424.90 ± 589.22, 74.95 ± 19.38-586.84 ± 194.49 h·ng·mL^-1, respectively. The plasma concentrations of the other four components (CC, BBR, BN, MCN) were below the detection limit. Three robust quantitative analytical methods were established and applied to evaluate variations of the content and in vivo exposure levels of 11 components in six ANP commercial products. The results demonstrated that the contents and in vivo exposure of some of the 11 components are consistent in the 6 products, particularly in the products containing the same natural or artificial bezoar and musk, or those manufactured by the same company. However, the inconsistency of the contents and in vivo exposure of some other ingredients suggests variations in the selection of raw herb medicines or processing technology. It suggests the crucial importance to monitor the source and quality of the raw herb medicines, and unify the processing technology. Furthermore, this study provides the data and reference methods for the supervision and consistency evaluation of quality amongst the products.