•A quasi-targeted analysis method was developed for metabolite identification of OH-PAHs.•LC–QqQMS/MS, LC–QTOF-MS and LC–Q-Orbitrap-MS were used for quasi-targeted analysis.•Nineteen hydroxylation-related metabolites of PAHs in human urine were identified.•Metabolic pathways of PAHs in human body were proposed using naphthalene as an example.Metabolite identification is crucial for revealing metabolic pathways and comprehensive potential toxicities of polycyclic aromatic hydrocarbons (PAHs) in human body. In this work, a quasi-targeted analysis strategy was proposed for metabolite identification of monohydroxylated polycyclic aromatic hydrocarbons (OH-PAHs) in human urine using liquid chromatography triple quadruple mass spectrometry (LC–QqQ-MS/MS) combined with liquid chromatography high resolution mass spectrometry (LC–HRMS). Potential metabolites of OH-PAHs were preliminarily screened out by LC–QqQ-MS/MS in association with filtering in a self-constructed information list of possible metabolites, followed by further identification and confirmation with LC–HRMS. The developed method can provide more reliable and systematic results compared with traditional untargeted analysis using LC–HRMS. In addition, data processing for LC–HRMS analysis were greatly simplified. This quasi-targeted analysis method was successfully applied to identifying phase I and phase II metabolites of OH-PAHs in human urine. Five metabolites of hydroxynaphthalene, seven of hydroxyfluorene, four of hydroxyphenanthrene, and three of hydroxypyrene were tentatively identified. Metabolic pathways of PAHs in human body were putatively revealed based on the identified metabolites. The experimental results will be valuable for investigating the metabolic processes of PAHs in human body, and the quasi-targeted analysis strategy can be expanded to the metabolite identification and profiling of other compounds in vivo.

•PFOA and PFOS were analyzed in cooking oil and pig adipose tissue.•A rapid and simple one-step reversed-phase liquid–liquid extraction was used for pretreatment.•LC–MS/MS method was developed and validated for the analysis of PFOA and PFOS.•The partition theory of PFOA and PFOS in extraction solution systems was discussed.•This method has been successfully applied to the analysis of PFOA and PFOS in real samples.Perfluorooctanoic acid (PFOA) and perfluorooctane sulfonic acid (PFOS) are two perfluorinated compounds (PFCs) ubiquitously present in the environment, which could pose potential adverse effects on human health. Contamination and presence of PFOA and PFOS should be eliminated or rigidly restricted in food stuffs such as cooking oils and lard (from pig adipose tissue). This work describes a rapid, simple, reliable and sensitive method for quantitative analysis of PFOA and PFOS in cooking oils and pig adipose tissue with liquid chromatography tandem mass spectrometry (LC–MS/MS). The pretreatment mainly included a one-step reversed-phase liquid–liquid extraction using the mixture of basified water/methanol as the aqueous system, and dichloromethane (DCM) as the non-polar system. PFOA and PFOS can be successfully separated from the two lipid-rich matrices, i.e., cooking oil and adipose tissue, and extracted into the aqueous system, and then directly analyzed with LC–MS/MS. This method was validated in terms of accuracy (both intra- and inter-batch), precision, recovery, linearity, sensitivity and applicability. The intra-batch accuracies for PFOA and PFOS in cooking oil samples were within 93.9–101.9% with relative standard deviation (RSD) no more than 10.9%, and the inter-batch accuracies were 91.2–96.2% with RSD not exceeding 10.0%. The intra-batch accuracies of the analytes in pig adipose tissue samples were 102.9–113.0% with RSD of 8.8–13.1%. And the quantification ranges of PFOA and PFOS were 0.01–25 ng/mL. This method has been applied to the analysis of PFOA and PFOS in real samples collected from local markets in Guangzhou, China.

This paper describes a method for the determination of platinum derived from cisplatin in human plasma ultrafiltrate using liquid chromatography tandem mass spectrometry (LC-MS/MS). Cisplatin and the internal standard trans-diamminedichloropalladium(II) (TDPD) were chelated with diethyldithiocarbamate (DDTC) and separated with an isocratic elution on a C18 column. The method was validated with intra-/inter-batch accuracy and precision (relative standard deviation, RSD, %), matrix effect, specificity, limit of quantification (LOQ), linearity and stability. The linear range was 1.0–100.0 ng mL−1 and the LOQ was 1.0 ng mL−1. The intra-/inter-batch accuracy and precision were 92.2–111.0%/94.7–106.0% and 3.9–8.8%/2.1–9.3%, respectively. This sensitive and interference-free method can permit reliable and accurate analysis of platinum derived from cisplatin in human plasma ultrafiltrate.

This paper describes a method for the determination of platinum derived from cisplatin in human plasma ultrafiltrate using liquid chromatography tandem mass spectrometry (LC-MS/MS). Cisplatin and the internal standard trans-diamminedichloropalladium(II) (TDPD) were chelated with diethyldithiocarbamate (DDTC) and separated with an isocratic elution on a C18 column. The method was validated with intra-/inter-batch accuracy and precision (relative standard deviation, RSD, %), matrix effect, specificity, limit of quantification (LOQ), linearity and stability. The linear range was 1.0–100.0 ng mL−1 and the LOQ was 1.0 ng mL−1. The intra-/inter-batch accuracy and precision were 92.2–111.0%/94.7–106.0% and 3.9–8.8%/2.1–9.3%, respectively. This sensitive and interference-free method can permit reliable and accurate analysis of platinum derived from cisplatin in human plasma ultrafiltrate.