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Benzophenone-type ultraviolet filters (BP-UVFs) are a group of emerging contaminants, which found in various environmental aqueous samples raising potential risks for public health concern and could bioaccumulate in the food chain. This study describes a simple and "green" method to rapidly analyze five BP-UVFs that are frequently found in surface water and in seawater samples. Dispersive solid-phase extraction (DSPE) using a zeolitic imidazolate framework­8 (ZIF-8) as the sorbent was applied to efficiently extract the BP-UVFs from aqueous samples, and they were then detected and quantified by UHPLC-electrospray ionization (+)-quadrupole time-of-flight mass spectrometry (UHPLC-ESI (+)-QTOF-MS). The ZIF-8 sorbent was synthesized by a green one-step mechanochemical process using water-assisted grinding and a stoichiometric reaction. The Box-Behnken Design coupled with the response surface method was applied to optimize the main DSPE extraction factors. The developed method was fully validated, showing low limits of quantification (LOQs; 0.3-20 ng L-1), satisfactory mean spiked recoveries (72-105%), and a high level of precision (3-9%). A preliminary analysis of the surface water and seawater samples revealed that 2-hydroxy-4-methoxybenzophenone (BP-3) was the most common BP-UVF present in our aquatic environment, likely due to its widespread applications and slow rate of degradation.

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Benzotriazole (BTRs) and benzothiazole (BTHs) derivatives are a group of high production volume chemicals with emerging health concern, which found in tea beverages raising potential risks for food safety and human health. The present work describes a simple method using a "green" deep eutectic solvent (DES) based-ultrasound-assisted liquid-phase microextraction (UALPME) to rapidly extract BTRs and BTHs from tea beverages, and then applying UHPLC-electrospray ionization (+)-quadrupole time-of-flight mass spectrometry for detection and quantification. To overcome the challenges related to different experimental conditions, a Factorial Multilevel Categoric Design and a Face Centered Central Composite Design were applied to screen and optimize the parameters for the DES-UALPME procedure, respectively. After optimization, the method was validated and shown to possess low limits of quantification (LOQs; 1.5-12 ng mL-1), high precision (3-13%), and satisfactory accuracy (65-107%). The developed method was then successfully applied for the analysis of some selected BTRs and BTHs in tea beverages.

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Benzotriazole (BTRs) and benzothiazole (BTHs) derivatives have been classified as high production volume pollutants of emerging concern. The present work describes a rapid and simple process using an eco-friendly deep eutectic solvent (DES) based-ultrasound-assisted liquid-liquid microextraction (DES-UALLME) technique to effectively extract five BTRs and four BTHs in human urine samples, and then applying ultrahigh-performance liquid chromatography and electrospray ionization (+)-quadrupole time-of-flight mass spectrometry (UHPLC-ESI(+)-QTOF-MS) for their detection and quantification. DESs are a group of novel "green" solvents, and their applications in sample pretreatment are appropriate for the requirements for green chemistry, environmental protection and sustainable development. Furthermore, to overcome the challenges related to different experimental conditions, multivariate experimental design approaches conducted by means of a multilevel categorical design and a Box-Behnken Design were applied to screen and optimize parameters that have significant influences on the extraction efficiency of DES-UALLME. After optimization, the method was validated and shown to possess low limits of quantitation (LOQs; 0.4 - 9 ng mL-1), high precision (3-12%), and high accuracy (mean spiked recoveries; 80-101%). The developed method was then successfully applied for the analysis of BTRs and BTHs in human urine samples. Interestingly, 5,6-dimethyl-1H-benzotriazole (XTR) was detected in almost all of the urine samples, which correlates with its high production and widely applications in industry processes and consumer products in Taiwan. These target analytes could potentially be used as biomarkers to assess exposure of BTRs and BTHs in biomonitoring programs and studies.

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This work describes a rapid solvent-minimized process to effectively determine four common paraben preservatives (methyl-, ethyl-, propyl- and butyl-paraben) in surface water samples. The method involved the use of a combination of a novel ultrasound-assisted simultaneous-silylation within dispersive liquid-liquid microextraction (UASS-DLLME) with detection by gas chromatography-tandem mass spectrometry (GC-MS/MS). To overcome the challenges related to the different experimental conditions, multivariate experimental design approaches conducted by means of a multilevel categorical design and a Box-Behnken design were utilized to screen and optimize parameters that have significant influences on the efficiency of silylation and extraction. The method was then validated and shown to provide low limits of quantitation (LOQs; 1-5 ng L-1), high precision (3-11%), and satisfactory mean spiked recoveries (accuracy; 79-101%). Upon analyzing samples of surface water obtained from the field, we found that, in total, there was a relatively high concentration of the target parabens ranging from 200 to 1389 ng L-1. The sources of the elevated levels of these parabens may be from the release of untreated municipal wastewater in this region, and also due to the widespread application of parabens in personal care and food products.

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This work describes a simple and environmental-friendly method for the simultaneous determination of five benzotriazole derivatives (BTRs) and four benzothiazole derivatives (BTs) that are frequently found in surface water. The target analytes were efficiently extracted from water samples using a "green" deep eutectic solvent (DES) as the extraction solvent based- ultrasound-assisted emulsification microextraction (DES-USAEME), and their determination were performed by ultrahigh-performance liquid chromatography and electrospray ionization (+)-quadrupole time-of-flight mass spectrometry (UHPLC-ESI(+)-QToF-MS). The DES was composed of a mixture of choline chloride and phenol (molar ratio 1:2). The DES-USAEME factors were optimized by a Box-Behnken Design coupled response surface methodology. The developed method was validated, providing limits of quantitation (LOQs; 02 µg L-1), high precisions (1-8%), and satisfactory mean spiked recoveries (72-104 %). Relatively high total concentrations of the target analytes were found in samples collected from a reservoir (47.2-101.3 µg L-1), which may have been released from tire-wear particles and scrap tires from buses and old tires that were strung alongside the shuttle boats to prevent the boats from coming into contact with each other or from impacting against the dock during docking. This is the first study on the occurrence of BTRs and BTs in reservoir samples.

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Exposure to environmental chemicals with oestrogenic effects has been associated with the development of endometrial cancer (EMCa). EMCa has become the most commonly diagnosed cancer of the female genital tract. To further understand the potential association between exposure to environmental endocrine disruptors and the occurrence of EMCa, we performed a case-control study between 2011 and 2014. We aimed to detect and compare concentrations of a known hormone disruptor, alkylphenol, between women diagnosed with either EMCa or uterine leiomyoma, and those who did not have either of these. Subjects were women diagnosed with either EMCa or uterine leiomyoma (LM) and healthy controls. A structured questionnaire was administered to collect information on lifestyle and health status. Gas chromatography/mass spectrometry was used to measure urinary NP and OP concentrations in participants. Multiple regression analysis was used to examine the association between exposure and outcomes. Overall, 397 women were recruited, including 49 with EMCa, 247 with LM, and 101 controls. Among them, 73.6% showed detectable levels of NP and 61.0% showed detectable levels of OP. The EMCa group had a significantly higher NP concentration than the control group. Higher OP concentrations were also found in participants with EMCa than those with LM and controls. In addition, women in the upper tertile of the NP group had a significantly increased risk of EMCa occurrence (odds ratio [95% confidence interval] = 4.47 [1.69-11.84] for EMCa vs. control). The same was found in the group of women with more than the median level of OP (odds ratio [95% confidence interval] = 4.32 [2.01-9.30] for EMCa vs. LM). Stratification of pre- and post-menopausal groups resulted in a similar association. The results show that NP/OP exposure is associated with EMCa. Further investigations and exposure minimisation are suggested.

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Benzotriazoles (BTRs) and benzothiazoles (BTs) are two groups of emerging concern and high production volume contaminants. Via the biomagnification of the food web, they could jeopardize human health. In this work, rapid determining the presence of five BTRs and two BTs in marketed fish was performed by a novel double-vortex-ultrasonic assisted matrix solid-phase dispersion (DVUA-MSPD) and UHPLC-electrospray ionization (+)-quadrupole time-of-flight mass spectrometry detection. Unlike traditional MSPD, we simplified the method without the use of mortar/pestle and SPE-column procedures. The DVUA-MSPD factors were screened by a multilevel categorical design, and then optimized by Box-Behnken Design plus with response surface methodology. The limits of quantification were 0.15-2 ng g-1 (dry weight). The satisfactory average recovery ranged from 70% to 93% with RSDs less than 9%. The developed method was successfully applied for the rapid determination of selected BTRs and BTs in fish samples at trace-level.

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The extensive use of preservatives during the growth, transport and storage of vegetables has been a concern because of their known or suspected toxicity that jeopardizes human health. This paper reports the development of a technique that rapidly determines the presence of five paraben preservative residues in leafy vegetables using double-vortex-assisted matrix solid-phase dispersion (DVA-MSPD) and UHPLC-electrospray ionization(-)-quadrupole time-of-flight mass spectrometry detection. We simplified the original MSPD technique by eliminating the use of mortar/pestle and SPE-column procedures. The DVA-MSPD factors were screened by a multilevel categorical design, and then optimized by Box-Behnken Design plus response surface methodology. The limits of quantification were 1.2-1.8 ng g-1 (dry weight). The satisfactory average recoveries were 85-104% with RSDs less than 10%. The developed method was successfully employed for the rapid determination of selected paraben residues at trace-level in leafy vegetable samples.

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A reliable and straightforward method was developed for the rapid determination of nine parabens (methyl-, ethyl-, propyl-, butyl-, isopropyl-, isobutyl-, pentyl-, hexyl-, and benzyl-parabens) in indoor dust by a mortar/pestle-free and column-free dual-vortex-assisted matrix solid-phase dispersion (DVA-MSPD) technique. After that, they were determined by isotope-dilution ultrahigh-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (UHPLC-qTOF-MS, or called UHPLC-HRMS) and operating in negative electrospray ionization mode. Optimization of the DVA-MSPD was done using Box-Behnken Design along with response surface methodology. Validation was done by measuring and calculating selectivity, limits of detection (LOD), limits of quantitation (LOQs), precision and trueness (accuracy) of intra- and inter-day analysis. The LOQs of the method ranged from 0.9 to 2.8 ng/g. High precisions for both intra- and inter-day analysis were obtained ranging from 1 to 8%. Excellent trueness (or mean extraction recovery) varied from 93 to 104%. The DVA-MSPD combined with isotope-dilution UHPLC-qTOF-MS was successfully applied to determine parabens in indoor dust samples from office rooms and private houses, and the total concentrations ranged from 55 to 686 ng/g.

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Rapid screening of two microcystins (i.e., microcystin-YR (MC-YR) and microcystin-LR (MC-LR)) in surface water samples was performed by a simple and eco-friendly procedure using deep eutectic solvent-based vortex-assisted liquid-liquid microextraction (DES-based VALLME) combined with ultrahigh-performance liquid chromatography and electrospray ionization (+)-quadrupole time-of-flight mass spectrometry (UHPLC-ESI(+)-qTOF-MS) detection. To obtain an efficient water-miscible DES, choline chloride and phenol at a molar ratio of 1 : 2 were used as an extractant for VALLME. To optimize factors of DES-based VALLME, response surface design alongside Box-Behnken design was used. The limits of quantitation (LOQs) were 0.5 ng mL-1 and 0.4 ng mL-1 for MC-YR and MC-LR, respectively, which is sensitive enough to meet the World Health Organization (WHO) maximum guideline level for MC-LR in water of 1.0 ng mL-1. Moreover, satisfactory precision with relative standard deviations (RSD) for both intra- and inter-day analysis lower than 11%, and trueness (also known as mean extraction recovery) ranged from 85.5 to 113% based on the ICH method validation guideline.

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An effective method to rapidly determine the presence of seven unmetabolized synthetic musks in human urine samples is developed. The target musks are five synthetic polycyclic musks (i.e., celestolide (ADBI), phantolide (AHMI), traseolide (ATII), galaxolide (HHCB), tonalide (AHTN)), and two nitro-aromatic musks (i.e., musk xylene (MX) and musk ketone (MK)). The method involved an ultrasound-assisted emulsification microextraction (USAEME) coupled with gas chromatography-mass spectrometry (GC-MS). The factors that affect USAEME efficiency were optimized in detail, and the optimized procedure involved the rapid injection of 50 µL of carbon tetrachloride into 1.0 mL of urine sample (contained 0.1-g of sodium chloride) in a conical bottom glass tube. After 1.0 min ultrasonication and 3 min centrifugation (at 7000 rpm), the sedimented extract 10 µL was directly injected into the GC-MS system. The limits of quantitation (LOQs) varied from 0.1 to 0.5 ng/mL. The precisions for both repeatability and reproducibility were <8%. The trueness varied from 79 to 96% with the RSD ranging from 2 to 8%. The total concentrations of the seven unmetabolized target musks in collected human urine samples were in the range from 0.93 to 3.74 ng/mL. HHCB and AHTN were detected in all the collected samples, and the daily excretion doses were evaluated.

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An analytical method that utilizes isotope-dilution ultrahigh-performance liquid chromatography coupled with hybrid quadrupole time-of-flight mass spectrometry (UHPLC-QTOF-MS or called UHPLC-HRMS) was developed, and validated to be highly precise and accurate for the detection of nine parabens (methyl-, ethyl-, propyl-, isopropyl-, butyl-, isobutyl-, pentyl-, hexyl-, and benzyl-parabens) in human urine samples. After sample preparation by ultrasound-assisted emulsification microextraction (USAEME), the extract was directly injected into UHPLC-HRMS. By using negative electrospray ionization in the multiple reaction monitoring (MRM) mode and measuring the peak area ratios of both the natural and the labeled-analogues in the samples and calibration standards, the target analytes could be accurately identified and quantified. Another use for the labeled-analogues was to correct for systematic errors associated with the analysis, such as the matrix effect and other variations. The limits of quantitation (LOQs) were ranging from 0.3 to 0.6 ng/mL. High precisions for both repeatability and reproducibility were obtained ranging from 1 to 8%. High trueness (mean extraction recovery, or called accuracy) ranged from 93 to 107% on two concentration levels. According to preliminary results, the total concentrations of four most detected parabens (methyl-, ethyl-, propyl- and butyl-) ranged from 0.5 to 79.1 ng/mL in male urine samples, and from 17 to 237 ng/mL in female urine samples. Interestingly, two infrequently detected pentyl- and hexyl-parabens were found in one of the male samples in this study.

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An analytical method that utilizes isotope-dilution gas chromatography-mass spectrometry (ID-GC-MS) coupled with injection-port butylation was developed. The method was validated, and confirmed to be able to determine the presence of three commonly detected endocrine-disrupting chemicals (EDCs: 4-tert-octylphenol (4-t-OP), 4-nonylphenols (4-NPs) and bisphenol A (BPA)) in human urine with high precision and accuracy. After sample preparation by solid-phase extraction, the extract was introduced into GC-MS via injection-port butylation. The butylated target analytes were identified and quantified by using ion-trap mass spectrometry operating in the selected-ion-storage mode, and employing the measurement of peak area ratios of the butylated target analytes and labeled-analogues in the samples and calibration standards. The labeled-analogues were also used to correct the variations associated with the analysis and matrix effect. The limits of quantitation (LOQs) ranged from 0.1 to 0.3ng/mL. High precisions for both intra- and inter-day analysis ranged from 1 to 6%, and excellent accuracy (mean recovery) ranged from 92 to 105% on two concentration levels. In human urine, the total concentrations of three selected EDCs varied from 1.28 to 7.14ng/mL. 4-NPs were detected within all collected samples. The developed method allows accurate analysis of trace-level of EDCs in urine, and these target EDCs could act as useful biomarkers to assess exposure in biomonitoring studies and programs.

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An effective and solvent-less method for the rapid determination of four commonly detected parabens (methyl-, ethyl-, propyl- and butyl-) in human urine samples is described. This method employed ultrasound-assisted emulsification microextraction (USAEME) before identification and quantitation of the parabens via on-line acetylation gas chromatography-mass spectrometry (GC-MS). Urine samples were enzymatically de-conjugated with ß-glucuronidase and then extracted by an optimal USAEME procedure for the measurement of total concentrations of target analytes. The optimal USAEME parameters for one mL of urine sample (containing 0.1-g of sodium chloride), according to the Box-Behnken design method, are thus described: extractant of 200-µL of ethyl acetate, and ultrasonication for 1.0min and centrifugation at 7000rpm (3min). The supernatant was collected and evaporated until dry. Then the residue was re-dissolved in methanol (100-µL), and the extract was subjected to on-line acetylation GC-MS analysis. The limits of quantitation (LOQs) were less than 0.06ng/mL. Precisions for both intra- and inter-day analysis were calculated, and were less than 8%. Mean extraction recovery (known as trueness) was between 83 and 101% on three concentration levels. In human urine, the total concentrations of the four selected parabens, according to preliminary results, range from 0.3 to 124.5ng/mL for male, and from 27.2 to 246.3ng/mL for female. Female urine samples showed higher concentrations for the target parabens, which may indicate higher exposure due to lifestyle. This method permits accurate and high-throughput analysis of parabens for epidemiological studies.

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A simple and effective method for determining short chain chlorinated paraffins (SCCPs) in indoor dust is presented. The method employed a modified vortex-homogenized matrix solid-phase dispersion (VH-MSPD) prior to its detection by gas chromatography - electron-capture negative-ion mass spectrometry (GC-ECNI-MS) operating in the selected-ion-monitoring (SIM) mode. Under the best extraction conditions, 0.1-g of dust sample was dispersed with 0.1-g of silica gel by using vortex (2min) instead of using a mortar and pestle (3min). After that step, the blend was transferred to a glass column containing 3-g acidic silica gel, 2-g basic silica gel, and 2-g of deactivated silica gel, used as clean-up co-sorbents. Then, target analytes were eluted with 5mL of n-hexane/dichloromethane (2:1, v/v) mixture. The extract was evaporated to dryness under a gentle stream of nitrogen. The residue was then re-dissolved in n-hexane (10µL), and subjected to GC-ECNI-MS analysis. The limits of quantitation (LOQs) ranged from 0.06 to 0.25µg/g for each SCCP congener. Precision was less than 7% for both intra- and inter-day analysis. Trueness was above 89%, which was calculated by mean extraction recovery. The VH-MSPD combined with GC-ECNI-MS was successfully applied to quantitatively detect SCCPs from various indoor dust samples, and the concentrations ranged from 1.2 to 31.2µg/g.

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An effective method for determining four commonly detected paraben preservatives (methyl, ethyl, propyl and butyl paraben) in marketed seafood is presented. This method employs matrix solid-phase dispersion (MSPD) before identification and quantification of the paraben preservatives via on-line acetylation gas chromatography-mass spectrometry (GC-MS). Parameters affecting the extraction efficiency of MSPD were optimized through a Box-Behnken design method. Under optimal condition, 0.5-g of freeze-dried seafood was mixed with 0.5-g of anhydrous sodium sulfate, and dispersed with 1.0-g of Florisil using vortex. After that, the blend was transferred to a glass column containing 1.5-g of silica gel+C18 (w/w, 9:1), which acted as clean-up co-sorbents. Then, target analytes were eluted with 12mL of acetonitrile. The extract was then derivatized on-line in the GC injection-port through reaction with acetic anhydride, and the identity and quantity of the target analytes were determined by the GC-MS system. The limits of quantitation (LOQs) were 0.2 to 1.0ng/g (dry weight). Preliminary results showed that the total concentrations of four selected parabens ranged from 16.7 to 44.7ng/g (dry weight).

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The rapid screening of trace levels of short-chain chlorinated paraffins in various aqueous samples was performed by a simple and reliable procedure based on vortex-assisted liquid-liquid microextraction combined with gas chromatography and electron capture negative ionization mass spectrometry. The optimal vortex-assisted liquid-liquid microextraction conditions for 20 mL water sample were as follows: extractant 400 µL of dichloromethane; vortex extraction time of 1 min at 2500 × g; centrifugation of 3 min at 5000 × g; and no ionic strength adjustment. Under the optimum conditions, the limit of quantitation was 0.05 µg/L. Precision, as indicated by relative standard deviations, was less than 9% for both intra- and inter-day analysis. Accuracy, expressed as the mean extraction recovery, was above 91%. The vortex-assisted liquid-liquid microextraction with gas chromatography and electron capture negative ionization mass spectrometry method was successfully applied to quantitatively extract short-chain chlorinated paraffins from samples of river water and the effluent of a wastewater treatment plant, and the concentrations ranged from 0.8 to 1.6 µg/L.

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Benzophenone-3 (BP-3) is a widely used organic UV-filter compound. Despite the frequent occurrence of BP-3 in aquatic environments, little is known about its effect on fish behavior. The aim of this study was to investigate the endocrine disrupting effects of BP-3 in male fighting fish (Betta splendens) with a focus on agonistic behavior. Male fighting fish were exposed to 10, 100, and 1000 µg/L BP-3, as well as a solvent control (0.1% ethanol) and a positive control (100 ng/L 17α-ethynylestradiol, EE2), for 28 days. At the beginning and the end of exposure, standard length and body mass of the fish were measured for calculating the condition factor (CF). In addition, spontaneous swimming activity (total distance moved) and agonistic behavior (maximum velocity and duration of opercular display in front of a mirror) were also quantified. At the end of exposure, the fish gonads were sampled for gonadosomatic index (GSI) measurement and histology. After the exposure, CF was significantly decreased in the 1000 µg/L BP-3 groups. Spontaneous swimming activity was not affected. However, maximum velocity was significantly reduced in the EE2 and 1000 µg/L BP-3 treatments; duration of opercular display was significantly decreased in the EE2 and 10 and 1000 µg/L BP-3 treatments. GSI was not significantly different between groups. There was a slight but statistically significant decrease of relative proportion of mature spermatozoa in testicular tissue in the 100 µg/L BP-3 treatment. Collectively, our results demonstrate that BP-3 can disrupt agonistic behavior of male fighting fish, indicating the endocrine disrupting activity of this compound.

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The rapid screening of trace amounts of the nitrogenous disinfection by-products, haloacetamides (HAcAms), in drinking and swimming pool water was performed by a simple and reliable procedure based on salt-assisted liquid-liquid extraction (SALLE) combined with injection-port silylation gas chromatography-mass spectrometry (IPS-GC-MS) method. The optimal SALLE conditions involved the injection of 4-mL of ethyl acetate into a 10-mL water sample (pH 7) containing 3-g of sodium sulfate. After vortex extraction for 1min and centrifugation, 10µL of the extract (mixed with 1µL of MTBSTFA) was directly determined by IPS-GC-MS. The limits of quantitation (LOQs) were determined to be 0.03-0.3µg/L. Precision, as indicated by relative standard deviations (RSDs), was less than 10% for both intra- and inter-day analysis. Accuracy, expressed as the mean extraction recovery, was between 76% and 94%. The SALLE plus IPS-GC-MS was successfully applied to quantitatively determine HAcAms from drinking and swimming pool water samples, and the total concentrations of the compounds ranged from 0.43 to 4.03µg/L.

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A solvent-free method for the rapid analysis of six benzophenone-type UV absorbers in water samples is described. The method involves the use of dispersive micro solid-phase extraction (DmSPE) followed by the simultaneous silylation and thermal desorption (SSTD) gas chromatography-mass spectrometry (GC-MS) operating in the selected-ion-storage (SIS) mode. A Plackett-Burman design was used for screening and a central composite design (CCD) for optimizing the significant factors was applied. The optimal experimental conditions involved immersing 1.5mg of the Oasis HLB adsorbent in a 10mL portion of water sample. After vigorous shaking for 1min, the adsorbents were transferred to a micro-vial, and were dried at 122°C for 3.5min, after cooling, 2µL of the BSTFA silylating reagent was added. For SSTD, the injection-port temperature was held at 70°C for 2.5min for derivatization, and the temperature was then rapidly increased to 340°C to allow the thermal desorption of the TMS-derivatives into the GC for 5.7min. The limits of quantitation (LOQs) were determined to be 1.5-5.0ng/L. Precision, as indicated by relative standard deviations (RSDs), was equal or less than 11% for both intra- and inter-day analysis. Accuracy, expressed as the mean extraction recovery, was between 87% and 95%. A preliminary analysis of the municipal wastewater treatment plant (MWTP) effluent and river water samples revealed that 2-hydroxy-4-methoxybenzophenone (BP-3) was the most common benzophenone-type UV absorber present. Using a standard addition method, the total concentrations of these compounds ranged from 5.1 to 74.8ng/L.

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