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To date, knowledge of internal human exposure to BPA and its analogues (particularly bisphenol S and bisphenol F, etc.) remains limited. In the present study, a method involving dispersive solid-phase extraction and LC/MS was proposed to investigate the contamination levels of 28 precursor bisphenols and 9 major metabolites in serum. The critical variables of preparation method were screened out by Plackett-Burman design and further optimized by central composite design. Left in optimal conditions, a total of 286 samples consisting of 153 males and 133 females were analyzed. The results showed that BPA dominated over all the cases with the highest positive rate (82.2% of all the surveyed people), and totally four metabolites (BPA β-D-glucuronide, BPA monosulfate, BPA bis-(β-D-glucuronide) and BPS monosulfate) were detectable. The occurrence of BPA bis-(β-D-glucuronide) in serum is reported for the first time and its higher positive rate and contamination concentrations suggested that it may be a more important metabolite of BPA than others. Negligible potential risk of health effects to blood donors was observed, since the estimated exposure levels (mean 32.1 ng/kg bw/day, 95th 123.2 ng/kg bw/day) were well below far less than the temporary tolerable reference dose of BPA that recommended by the European Food Safety Authority (4 μg/kg bw/day by). The reference level of BPA for healthy population was determined to be 4.09 μg/L via the percentile method.

To address problems such as environmental accumulation, improved methods are required for the detection and analysis of fluoroquinolones. Herein, we prepared a surface molecularly imprinted polymer (MIP) based on dopamine-coated magnetic nanoparticles. The performance of this MIP as a novel adsorbent for fluoroquinolones was analyzed using high-performance liquid chromatography. Furthermore, the morphology and physicochemical properties of the prepared material were characterized by Fourier transform infrared spectroscopy, transmission electron microscopy, thermogravimetric analysis, Brunauer–Emmett–Teller surface area analysis, and vibrating sample magnetometry. The synthesized molecules consisted of a core–shell constitution with a Fe3O4 nucleus and a polydopamine enclosure, the surface of which was imprinted using gatifloxacin as a template molecule. The obtained polymers had a high specific surface area, good superparamagnetism, and excellent selectivity of the target molecules. Under optimal adsorption conditions, the ultimate loading capacity of gatifloxacin on the MIP was 51.9 mg/g, with an equilibrium adsorption time of 30 min and an imprinting factor of 2.24. After six cycles, the adsorption capacity of this adsorbent did not decrease significantly. For the analytical characteristics of the method, we inserted the application part of the sample in the local river water. Through the spiked recovery of the three FQs aqueous solutions, it was found that their spiked recovery, LOD, and LOQ were 84.1–91.9%, 6.4–9.9 ng mL−1, and 17.8–34.5 ng mL−1, respectively. Owing to its adsorption selectivity and recyclability, this magnetic MIP is a promising adsorbent for sample separation and pretreatment applications.

In this paper, a novel and recyclable amino-functionalized nano-composite material (NCM) using tetraethylenepentamine (TEPA) as a coupling agent was synthesized. The properties of the TEPA-NCM were characterized by transmission electron microscopy (TEM), Fourier transform infrared analysis (FTIR), thermogravimetric analysis (TGA) and elemental analysis (EA). An effective dispersive solid-phase extraction (dSPE) procedure using the TEPA-NCM was developed, and comparative studies were carried out among Carbon/NH2 SPE, primary secondary amine (PSA) dSPE and TEPA-NCM dSPE. The results showed that TEPA-NCM dSPE was faster, easier and more effective to clean and enrich than the Carbon/NH2 cartridges, and the TEPA-NCM was much more effective to remove the pigments in vegetable samples than the PSA materials. The TEPA-NCM could be reused at least five times without much sacrifice of the cleanup efficiency. Furthermore, a gas chromatography–triple quadrupole mass spectrometry (GC–QqQ-MS/MS) method was established for the simultaneous determination of 29 pesticides (such as organochlorine and organophosphorus pesticides) in vegetables by dSPE using acetonitrile as an extraction solvent and TEPA-NCM as an adsorbent instead of PSA. The recoveries were in the range of 75–114% for all analytes except for trans-chlordane. The RSDs were in the range of 2–17%. The linearities were in the range of 0.4–100.0 μg/kg with determination coefficients (r2) higher than 0.986 for all compounds. The limits of detection (LODs) for all pesticides were less than 0.29 μg/kg and the limits of quantification (LOQs) were between 0.17 and 0.95 μg/kg. The developed method was applied to fifteen real vegetable samples, and it was confirmed that the TEPA-NCM was one of a kind of highly effective dSPE materials used for the pesticides analyses.

A novel, sensitive, and accurate method has been successfully developed for the simultaneous determination of 3 monochlorophenols (MCPs) in drinking water samples by ion chromatography (IC) coupled with atmospheric pressure chemical ionization mass spectrometry in the negative mode. Drinking water was preconcentrated by solid-phase extraction (SPE). The IC separation was carried out with an IonPac® AS18 analytical column (250 mm × 4.0 mm) and an IonPac® AG18 guard column (50 mm × 4.0 mm) using 15 mmol l −1 KOH containing 10% acetonitrile as mobile phase in the isocratic mode at a constant flow rate of 1.0 ml min −1 . The molecular ion m/z 127 [M-H] was selected for the quantification in the selected ion monitoring (SIM) mode. Within-the-day and day-to-day relative standard deviations were less than 8.6 and 10.5%, respectively. The limits of quantification (LOQs) in water samples were 0.02, 0.01, and 0.01 μg l −1 for 2-MCP, 3-MCP, and 4-MCP, respectively. The method allows the three target compounds in water samples to be determined at a level of ng ml −1 , and it has been successfully applied to the routine analyses.