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Abstract We used a hybrid precipitation method to simultaneously extract and analyze 24 personal care products (PCPs), including 16 biocides, 4 synthetic musks, and 4 benzotriazoles, in the plasma of fish. The method's performance was validated for plasma samples with and without β -glucuronidase/aryl-sulfatase hydrolysis. The recoveries were in the range of 70–120% for most of the PCPs, except N , N -diethyl-3-methylbenzamide (DEET), clotrimazole (CTZ), miconazole and itraconazole at spiking concentration of 20 and 5 ng/mL. The quantification limits ranged between 0.89 and 17.9 ng/mL (hydrolyzed plasma) and 0.85–18.5 ng/mL (non-hydrolyzed plasma), except CTZ at 77.5 ng/mL and 76.3 ng/mL. Totally, 13 PCPs were detected in plasma samples of fish collected from the Yangtze River, with a maximum concentration of 58.4 ng/mL (galaxolide). Compounds with the phenol hydroxyl groups of parabens or triclosan in hydrolyzed plasma showed higher concentrations than those in unhydrolyzed plasma with the ratio of conjugation (glucuronides + sulfates) forms up to 86%. The median values for the logarithm of bioaccumulation factors were between 1.39 and 4.15, which were 2–3 orders of magnitude higher than the theoretical logarithm of bioconcentration factors. Using the fish plasma model, the effect ratios (effect concentration/measured plasma concentration ratios) of tonalide, galaxolide, benzotriazole, triclosan, and DEET reached 0.35, 4.15, 3.78, 7.52, and 9.24, respectively. These are recognized as priority chemicals for further risk assessment. Graphical abstract Unlabelled Image Highlights • A method was developed to determine personal care products (PCPs) in fish plasma. • The MQLs of most PCPs ranged at 0.85–18.5 ng/mL (except clotrimazole at 77.5 ng/mL). • Thirteen PCPs were detected in plasma from fish collected from the Yangtze River. • Parabens and triclosan with OH group showed high ratio of conjugation up to 86%. • Five PCPs are recognized as the priority attended chemicals. [ABSTRACT FROM AUTHOR]