Fabrication of carboxymethyl chitosan–hemicellulose resin for adsorptive removal of heavy metals from wastewater

Carboxymethyl chitosan–hemicellulose resin(CMCH) was synthesized by thermal cross-linking process and characterized by FTIR, TGA, and SEM. Subsequently, the adsorption properties of CMCH toward Ni(Ⅱ),Cd(Ⅱ), Cu(Ⅱ), Hg(Ⅱ), Mn(Ⅶ) and Cr(Ⅵ) were evaluated. Various factors affecting the uptake behavior such as pH, temperature, contact time and the initial concentration of the metal ions were investigated.The results showed that all adsorption processes fit the pseudo-second-order model and Langmuir isotherm equation. Significantly, the regeneration experiments showed CMCH can be used as a potentially recyclable and effective adsorbent for the removal and recovery of metal ions from wastewater.     

Determination of multi-class pharmaceuticals in wastewater by liquid chromatography–tandem mass spectrometry (LC–MS–MS)

An analytical method for multi-class pharmaceuticals determination in wastewater has been developed and validated. Target compounds were: sulfonamides (sulfadiazine, sulfaguanidine, sulfamethazine, sulfamethoxazole), fluoroquinolones (ciprofloxacin, enrofloxacin, norfloxacin), diaminopyrimidine (trimethoprim), anaesthetic (procaine), anthelmintic (praziquantel and febantel), and macrolide (roxithromycin). The method involves pre-concentration and clean-up by solid-phase extraction (SPE) using Strata-X extraction cartridges at pH 4.0. Target analytes were identified and quantitatively determined by liquid chromatography–tandem mass spectrometry using multiple reaction monitoring (MRM). Recoveries were higher than 50% with relative standard deviation (RSD) below 18.3% for three concentrations. Only for sulfaguanidine was low recovery obtained. Matrix effect was evaluated using matrix-matched standards. The method detection limit (MDL) was between 0.5 and 5 ng L⁻¹ in spiked water samples. The precision of the method, calculated as relative standard deviation, ranged from 0.5 to 2.0% and from 1.4 to 8.3 for intra-day and inter-day analysis, respectively. The described analytical method was used for determination of pharmaceuticals in effluent wastewaters from the pharmaceutical industry.     

TiO2–active carbon composites for wastewater photocatalysis

Titanium oxide–active carbon composites (TiO₂–AC) with photocatalytic activity were prepared by sol–gel method at low temperature. Titanium isopropoxide and active carbon were used as precursors, ethanol as solvent and HNO₃ as catalyst. The composition of the studied composites was accomplished by means of X-ray diffraction, and Fourier Transform-Infrared spectrometry. The rutile crystalline phase was present in all samples. In scanning electron microscopy images the TiO₂ aggregates existed either on the surface of the active carbon or heterogeneously dispersed over the whole catalyst matrix. The contact angle and point of zero charge measurements were applied to characterise the surface energy and surface charge. The photocatalytic activities of the TiO₂–AC composites were evaluated in the bleaching of methyl orange and methylene blue solution from ternary mixture of methyl orange, methylene blue and Triton X100. The double divisor ratio spectra derivative method (as a multivariable calibration method) was developed to overcome the spectral overlapping, for the simultaneous analysis of ternary mixture.     

Potential of Mg–Zn–Al layered double hydroxide (LDH)/montmorillonite nanocomposite in remediation of wastewater containing manganese ions

Research on Chemical Intermediates - A Mg–Zn–Al (LDH)/MMT nanocomposite was prepared by physical interaction between Mg–Zn–Al layered double hydroxide (LDH) and...     

Determination of 76 pharmaceutical drugs by liquid chromatography–tandem mass spectrometry in slaughterhouse wastewater

A multi-residue method for the analysis of 76 pharmaceutical agents of nine classes of drugs (tetracyclines, macrolides, fluoroquinolones, β-agonists, β-blockers, diuretics, sedatives, sulfonamides and chloramphenicol) in slaughterhouse wastewater and a receiving river is presented. After simultaneous extraction with an Oasis HLB solid-phase extraction (SPE) cartridge and further purification using an amino SPE cartridge, analytes were detected by liquid chromatography–electrospray ionization-tandem mass spectrometry in positive or negative ion mode. Standard addition was used for quantification to overcome unavoidable matrix effects during ESI-MS analysis. Recoveries for most analytes based on matrix-matched calibration in different test matrices were >60%. The method quantification limits of 76 pharmaceuticals were in the range 0.2–30 ng/L. Nineteen compounds of 76 drugs were found in raw and treated slaughterhouse wastewater from four main slaughterhouses in Beijing. Sulfanamides (sulfanilamide, sulfameter), fluoroquenones (ofloxacin, pefloxacin, norfloxacin, ciprofloxacin, enrofloxacin), tetracyclines (tetracycline, oxytetracycline) and macrolides (kitasamycin, tylosin, erythromycin) were most frequently detected, with the highest levels up to ∼3 μg/L in slaughterhouse wastewater and ∼1 μg/L in treated wastewater. Illicit drugs for animal feeding such as clenbuterol and diazepam were commonly detected in slaughterhouse wastewater. These analytes were also observed in a river receiving slaughterhouse wastewater, with a highest level of up to 0.2 μg/L.     

Cleanup strategies and advantages in the determination of several therapeutic classes of pharmaceuticals in wastewater samples by SPE–LC–MS/MS

This work describes the development and validation of an offline solid-phase extraction with simultaneous cleanup capability, followed by liquid chromatography–(electrospray ionisation)–ion trap mass spectrometry, enabling the concurrent determination of 23 pharmaceuticals of diverse chemical nature, among the most consumed in Portugal, in wastewater samples. Several cleanup strategies, exploiting the physical and chemical properties of the analytes vs. interferences, alongside with the use of internal standards, were assayed in order to minimise the influence of matrix components in the ionisation efficiency of target analytes. After testing all combinations of adsorbents (normal-phase, ion exchange and mixed composition) and elution solvents, the best results were achieved with the mixed-anion exchange Oasis MAX cartridges. They provided recovery rates generally higher than 60%. The precision of the method ranged from 2% to 18% and 4% to 19% (except for diclofenac (22%) and simvastatin (26%)) for intra- and inter-day analysis, respectively. Method detection limits varied between 1 and 20 ng L⁻¹, while method quantification limits were <85 ng L⁻¹ (both excluding ibuprofen). This analytical method was applied to gather preliminary results on influents and effluents of two wastewater treatment plants (WWTPs) located in the urban region of Porto (Portugal). Typically, paracetamol, hydrochlorothiazide, furosemide, naproxen, ibuprofen, diclofenac and bezafibrate were detected in concentrations ranging from 1 to 20 μg L⁻¹, while gemfibrozil, simvastatin, ketoprofen, azithromycin, bisoprolol, lorazepam and paroxetine were quantified in levels below 1 μg L⁻¹. These WWTPs were given particular attention since they discharge their effluents into the Douro river, where water is extracted for the production of drinking water. Some sampling spots in this river were also analysed.     

Calculation of viscosity–temperature curves for glass obtained from four wastewater treatment plants in Egypt

This article establishes the relationship between the chemical composition, temperature and viscosity of glasses obtained from the four sludge treatment plants of urban and industrial wastewater from the Nile Delta in Egypt. In order to determine the working conditions of these glasses and their growth temperature, different techniques have been used: differential thermal analysis, hot stage microscopy and dilatometry. We used a prototype of hot stage microscopy, with the help of an image analysis programme developed in the present study. The chemical composition of major oxides sludge ranging from: SiO₂ (36–48 wt%), Al₂O₃ (9–16 wt%), CaO (5–25 wt%), P₂O₅ (1.5–11 wt%), and Fe₂O₃ (~9 wt%), this composition is close to a basalt rock, being necessary to incorporate some raw materials to adjust it to the basalt rock that has a good viscosity-temperature curve. The glass transition temperatures of the four glasses obtained vary between 650 and 725 °C and the growth occurs between 938 and 1,033 °C. We also obtained the viscosity–temperature curves with the aid of the hot stage microscopy that has allowed us to determine the working temperatures of the four glasses, ranging from 926 to 1,419 °C, depending on the type of forming process used.     

Enantiomeric determination of azole antifungals in wastewater and sludge by liquid chromatography–tandem mass spectrometry

A sensitive and reliable liquid chromatographic-tandem mass spectrometric method for enantiomeric determination of five chiral azole antifungals (econazole, ketoconazole, miconazole, tebuconazole, and propiconazole) in wastewater and sludge has been established and validated. An isotope-labeled internal standard was used for quantification. Recovery of the individual enantiomers was usually in the range of 77-102 % for wastewater and 71-95 % for sludge, with relative standard deviations within 20 %. No significant difference (p>0.05) was observed between recovery of pairs of enantiomers of the chiral azole antifungals except for those of tebuconazole. Method quantification limits for individual enantiomers were 0.3-10 ng L(-1) and 3-29 ng g(-1) dry weight for wastewater and sludge, respectively. The method was used to investigate the enantiomeric composition of the azole pharmaceuticals in wastewater and sludge samples from a sewage treatment plant in China. Enantiomers of miconazole, ketoconazole, and econazole were widely detected. The results showed that the azole antifungals in wastewater and sludge were generally racemic or marginally non-racemic. The method is a useful tool for investigation of the enantiomeric occurrence, behavior, and fate of the chiral azole antifungals in the environment.     

One- and two-stage upflow anaerobic sludge-bed reactor pretreatment of winery wastewater at 4–10°C

The operating performance of a single and two (in series) laboratory upflow anaerobic sludge-bed (UASB) reactors (2.7-L working volume, recycle ratio varied from 1:1 to 1:18) treating diluted wine vinasse was investigated under psychrophilic conditions (4-10 degreesC). For a single UASB reactor seeded with granular sludge, the average organic loading rates (OLRs) applied were 4.7, 3.7, and 1.7 g of chemical oxygen demand (COD)/(L.d) (hydraulic retention times [HRTs] were about 1 d) at 9-11, 6 to 7, and 4 to 5 degreesC, respectively. The average total COD removal for preacidified vinasse wastewater was about 60% for all the temperature regimes tested. For two UASB reactors in series, the average total COD removal for treatment of non-preacidified wastewater exceeded 70% (the average OLRs for a whole system were 2.2, 1.8, and 1.3 g of COD/[L.d] under HRTs of 2 d at 10, 7, and 4 degreesC, respectively). In situ determinations of kinetic sludge characteristics (apparent Vm and Km) revealed the existence of substantial mass transfer limitations for the soluble substrates inside the reactor sludge bed. Therefore, application of higher recycle ratios is essential for enhancement of UASB pretreatment under psychrophilic conditions. The produced anaerobic effluents were shown to be efficiently posttreated aerobically: final effluent COD concentrations were about 0.1 g/L. Successful operation of the UASB reactors at quite low temperatures (4-10 degreesC) opens some perspectives for application of high-rate anaerobic pretreatment at ambient temperatures.     

Rapid determination of five antibiotic residues in swine wastewater by online solid-phase extraction–high performance liquid chromatography–tandem mass spectrometry

A simple and quick online solid-phase extraction (SPE) coupled to liquid chromatography (LC)/tandem mass spectrometry (MS/MS) for the determination of the five antibiotics (florfenicol, FF; lincomycin, LCM; oxytetracyclin, OTC; tylosin, TS; valnemulin, VLM) in swine wastewater has been developed. After filtration, aliquots (100 μl) of wastewater samples were directly injected to a column-switching LC system. Some matrix interference was removed by washing up SPE column with 0.2% formic acid solution and acetonitrile. Antibiotics eluted from SPE column were separated on analytical column by converting switching valve and were detected by MS/MS. Calibration curves using the method of standard addition had very good correlation coefficients (r > 0.99) in the range of 0.1 to 2 ng/ml. The intra-day precision of the method was less than 12% and the inter-day precision was between 6 to 17%. The detection limits were 0.01–0.1 ng/ml. When this method was applied to wastewater samples in swine facilities, four compounds (LCM, OTC, TS, and VLM) were detected.     

Quantitative determination of triclocarban in wastewater effluent by stir bar sorptive extraction and liquid desorption–liquid chromatography–tandem mass spectrometry

Triclocarban is an antimicrobial and antibacterial agent found in personal care products and subsequently is a prevalent wastewater contaminant. A quantitative method was developed for the analysis of triclocarban in wastewater effluents using stir bar sorptive extraction–liquid desorption (SBSE–LD) followed by liquid chromatography–tandem mass spectrometry (LC–MS/MS) by means of an electrospray interface. A stir bar coated with polydimethylsiloxane (PDMS) is placed within a vial containing wastewater effluent and is stirred for an hour at room temperature. The PDMS stir bar is then placed in a LC vial containing methanol and is desorbed in a sonicator bath. The methanol is evaporated to dryness and reconstituted in 75% methanol. Spike and recovery experiments in groundwater that did not contain native concentrations of triclocarban were performed at 0.5 μg/L and were 93 ± 8%. Recoveries in wastewater effluent that were corrected for the background levels of triclocarban were 92 ± 2% and 96 ± 5%, respectively, when spiked with 0.5 and 5 μg/L of triclocarban. The precision of the method as indicated by the relative standard error was 2%. The limit of quantitation was 10 ng/L. The SBSE–LD–LC/MS/MS method was applied to wastewater effluent samples collected from northeast Ohio. Triclocarban was quantitated in all five effluent samples, and its concentration ranged from 50 to 330 ng/L. The described method demonstrates a simple, green, low-sample volume, yet, sensitive method to measure triclocarban in aqueous matrices.     

Determination of parabens in wastewater samples via robot-assisted dynamic single-drop microextraction and liquid chromatography–tandem mass spectrometry

Dynamic single-drop microextraction (SDME) was automatized employing an Arduino-based lab-made Cartesian robot and implemented to determine parabens in wastewater samples in combination with liquid chromatography–tandem mass spectrometry. A dedicated Arduino sketch controls the auto-performance of all the stages of the SDME process, including syringe filling, drop exposition, solvent recycling, and extract collection. Univariate and multivariate experiments investigated the main variables affecting the SDME performance, including robot-dependent and additional operational parameters. Under selected conditions, limit of detections were established at 0.3 µg/L for all the analytes, and the method provided linear responses in the range between 0.6 and 10 µg/L, with adequate reproducibility, measured as intraday relative standard deviations (RSDs) between 5.54% and 17.94%, (n = 6), and inter-days RSDs between 8.97% and 16.49% (n = 9). The robot-assisted technique eased the control of dynamic SDME, making the process more feasible, robust, and reliable so that the developed setup demonstrated to be a competitive strategy for the automated extraction of organic pollutants from water samples.     

An interlaboratory study of quantitation procedures for the analysis of water and wastewater for organo-chlorine pesticides by gas chromatography–electron capture detector

An interlaboratory study was conducted to assess two widely used procedures for estimating quantitation levels. Six laboratories participated in the analysis of artificially prepared water samples for organo-chlorine compounds by liquid-liquid extraction followed by gas chromatography–electron capture detector using USEPA Method 608. The study consisted of three phases, including six months of results from analyte free samples, the replicate analysis of fortified samples at a single concentration by the laboratory, and finally the analysis of blind fortified samples prepared by a third party. Estimated detection and quantitation limits (Currie's L_C and L_Q and USEPA's MDL and ML) were determined for each laboratory-method-analyte combination and then compared to the observed detection and quantitation limits. The overwhelming majority of analyte free samples had a reported value of zero. As a result, observed quantitation and detection limits were frequently zero. When they were not zero, the observed quantitation limits were sometimes less than the observed detection limits and when they were not, there was no observed fixed ratio between the quantitation and detection limits. The variability between days of analysis and the use of noise reducing techniques proved to be a significant source of the observed non-normal distribution of results from distilled water samples with a concentration of zero. Conventional procedures and their underlying analytical and statistical assumptions did not provide useful predictions of laboratory quantitation based upon the results of this study. Rather than one time statistical determinations, ongoing verification of quantitation limits may be a better approach.     

Gas–liquid chromatography–tandem mass spectrometry methodology for the quantitation of estrogenic contaminants in bile of fish exposed to wastewater treatment works effluents and from wild populations

Fish can be exposed to a complex mixture of chemical contaminants arising from the exposure to wastewater treatment works (WwTWs) effluents. Some of these contaminants are estrogenic and have been associated with feminisation of male fish and the presence of populations containing intersex individuals. However the detection of trace levels (ng/L) of estrogenic chemicals surface waters can be difficult and does not give information on the exposure of aquatic organisms to these contaminants. In this study we assessed whether the analysis of estrogenic substances that bioconcentrate in fish bile can be used to detect the exposure of fish to feminising contaminants in receiving waters and effluents, and thus facilitate their monitoring of these substances in aquatic environments. Estrogenic metabolites in bile were deconjugated using enzymatic hydrolysis and partially purified by solid phase extraction. Steroidal and xenoestrogens were derivatized to their trimethylsilyl ethers and quantified by gas–liquid chromatography–mass spectrometry (GC–MS/MS) using multiple reaction monitoring. The method was validated using spiked bile samples from immature female rainbow trout (Oncorhynchus mykiss) as well as bile from sexually mature roach (Rutilus rutilus) that had been exposed to either tap water or an undiluted estrogenic effluent for 10 days or captured from a river site downstream of a WwTWs effluent discharge. The mean recovery of target analytes from spiked bile was between 86 and 99% and the limit of detection was between 0.1 and 0.7 ng/mL bile for bisphenol A (BPA), 17β-estradiol (E2), estrone (E1) and 17α-ethinylestradiol (EE2), and 11, 60 and 327 ng/mL bile for branched nonyl chain isomeric mixtures of 4-nonylphenolethoxylate (NP1EO), 4-nonylphenol (NP) and 4-nonylphenoldiethoxylate (NP2EO), respectively. All target analytes were detected in bile from roach exposed directly to a WwTWs effluent, with concentrations between 6–13 μg/mL bile for NP, 18–21 μg/mL for NP1EO, 75–135 μg/mL for NP2EO, 0.7–2.5 μg/mL for BPA, E2 and E1 and 17–29 ng/mL for EE2. With the exception of NP2EO, all analytes were detected in at least 2 out of the 5 fish sampled from the River Thames. BPA and NP1EO were detected in all three reference fish held in tap water indicating possible contamination from laboratory plastics. The work shows that analysis of 20–100 μL quantities of bile could be a useful approach in detecting exposure to mixtures of estrogenic contaminants taken up by fish from WwTW effluents and has the potential for monitoring the efficacy of remediation strategies that may be adopted for reduction of these endocrine disrupting chemicals in the aquatic environment.     

Integrated procedure for multiresidue analysis of dissolved and particulate drugs in municipal wastewater by liquid chromatography–tandem mass spectrometry

For the first time, an integrated procedure for a quantitative multiresidue analysis of dissolved and particulate illicit drug target residues was developed and validated in three different wastewater matrices. The procedure consists of a comprehensive sample enrichment, fractionation and cleanup followed by the determination of target analytes by triple quadrupole liquid chromatography–tandem mass spectrometry in both positive and negative ionisation polarities. The enrichment of illicit drugs from suspended solids and aqueous samples was performed using pressurised liquid extraction and solid phase extraction (SPE), respectively. The performance of different SPE cartridges was investigated in order to optimise the overall recovery and to reduce the matrix effects. The optimal results were obtained by combining mixed cation exchange (Oasis MCX) cartridges for fractionated enrichment, weak anion exchange for an additional extract cleanup and optimised chromatographic separation to minimise the impact from co-extracted interferences. The method was applied for the analysis of raw wastewater (RW), activated sludge (AS) and secondary effluent (SE) samples collected at four different wastewater treatment plants. The average contributions of the particulate drugs in the RW and AS were 1–28 and 23–65 %, respectively. This suggested that the total mass loads of some drugs might be underestimated by neglecting the particulate fraction. Moreover, relatively high distribution coefficients, determined for 2-ethylidene-1,5-dimethyl-3,3-diphenylpyrrolidine (RW?=?1211 L/kg) and 11-hydroxy-Δ⁹-tetrahydrocannabinol (RW?=?1,786 L/kg) implied that adsorption might play a significant role in their overall removal during wastewater treatment.

Progresses on electrospun metal–organic frameworks nanofibers and their wastewater treatment applications

Metal–organic frameworks (MOFs) have been proven to be outstanding adsorbent materials which possess excellent pollutant removal performances in wastewater treatment. However, MOFs consumption, loss, or blockage in reactor pipelines as well as the long and complicated recycling process severely limit their practical applications. Therefore, construction of novel MOFs composites with extremely high ease-of-use property has become a research hotspot, such as two-dimensional (2D) MOFs fibrous membranes. In this review, the exploitation of MOFs nanofibrous membranes via electrospinning and their applications in wastewater treatment are summarized. The MOFs nanofibers (NFs) architectures are established systematically by five routes: (1) direct electrospinning of MOFs-polymer; (2) induced growth of MOFs on electrospun NFs containing seeds; (3) growth of MOFs on electrospun organic NFs’ (4) growth of MOFs on electrospun inorganic NFs; and (5) simultaneous electrospinning and electrospraying. Furthermore, the applications of different types of MOFs nanofibrous membranes and their derivatives in water treatment and purification are discussed, including oil-water separation, the removal of heavy metal ions, organic dyes, personal care products, non-steroidal anti-inflammatory drugs (NSAIDs) and so on. The adsorption properties and mechanisms of electrospun MOFs nanofibrous membranes towards various environmental pollutants are discussed. Finally, the challenges of electrospun MOFs NFs, the limitations of their applications, and future development trends are prospected.     

Zinc–aluminum layered double hydroxide as a nano-sorbent for removal of Reactive Yellow 84 dye from textile wastewater effluents

In this research, the zinc–aluminum layered double hydroxide (Zn–Al LDH) was synthesized and structurally and morphologically characterized by X-ray diffraction, Fourier transform infrared spectroscopy, transmission electron microscopy and N₂ adsorption–desorption techniques. The obtained nano-structured inorganic material was employed as an innovative nano-sorbent for separation of Reactive Yellow 84 (RY84) dye from aqueous solutions, which can be spectrophotometrically monitored at λ = 359 nm. The effect of several parameters such as type of interlayer anion in Zn–Al LDH structure, pH, sample flow rate, elution conditions, amount of nano-sorbent, sample volume and co-existing ions on the retention efficiency was investigated and optimized. The results showed that trace amounts of the RY84 could be retained using a column packed with 300 mg of the Zn–Al(NO₃ ^?) LDH at pH 8 and stripped by 2.5 mL of 3.0 mol L^?1 NaOH. Under the optimum experimental conditions, the limit of detection and the relative standard deviation were 0.04 μg mL^?1 and 1.8 %, respectively. The calibration graph using the presented solid phase extraction system was linear in the range of 0.15–1.5 μg mL^?1 with a correlation coefficient of 0.9982. The method was successfully applied to removal of RY84 from several textile wastewater effluents.     

Synthesis of core–shell magnetic ion-imprinted polymer nanospheres for selective solid-phase extraction of Pb2+ from biological,food, and wastewater samples

Magnetic ion-imprinted polymer nanospheres, which have core–shell structures, have been synthesized as an adsorbent for extraction of Pb²⁺ from real samples prior to its flame atomic absorption spectrometric determination. The prepared adsorbent has been characterized using XRD, VSM, TEM, and FTIR measurements. The optimization results revealed that the adsorbent exhibited high selectivity toward Pb²⁺ over other cations such as Cu²⁺ and Zn²⁺. In addition, the removal efficiency of synthesized adsorbent was considerable (q_m?=?171.42?mg g^?1), its calibration curve was linear (0.5?850.0?ng mL^?1), and detection limit was 0.01?ng mL^?1. These results suggested that the prepared nanoadsorbent is an ideal candidate for solid-phase extraction of Pb²⁺ ions.     

The graphene oxide/magnesium–aluminium bimetallic hydroxides composite used as solid-phase extractant for determination of monoaromatic hydrocarbons in wastewater

The graphene oxide (GO) and the magnesium–aluminium bimetallic hydroxides composite (GO/Mg-Al-LDH) was used as a solid-phase extractant for determination of toluene, ethylbenzene, p-xylene, m-xylene, o-xylene, 1,3,5-trimethylbenzene and 1,2,4-trimethylbenzene in wastewater by gas chromatography-mass spectrometry analytical method. When the amount of solid-phase extractant was 1.5 g, the extraction time was 6 min, and the elution with 2 mL of chloroform for 3 min, seven monoaromatic hydrocarbons (MAHCs) in 500 mL of water sample can be well extracted and separated. Under the optimised experimental conditions, the mass concentration of each component in the range of 0.01–5 ng/mL has a good linear relationship with the peak area, the coefficients of determination are all greater than 0.995. The relative standard deviation (n = 5) and the method detection limit range are 2.9–7.1% and 0.0005–0.005 ng/mL, respectively. The seven of MAHCs in Dongfengqu River and laboratory wastewater of Chengdu University of Technology can be effectively detected, the recovery rate and the relative standard deviation (n = 5) are 83.0–110.0% and 3.7–9.4%, respectively. For the first time, the GO/Mg-Al-LDH composite was used as a solid-phase extraction material, and seven MAHCs in water were successfully determined by GC-MS. The detection method is established with low detection limit and high reproducibility which can meet the measurement requirements of trace MAHCs in wastewater.