Development of a flow system for the determination of cadmium in fuel alcohol using vermicompost as biosorbent and flame atomic absorption spectrometry

In this study a method for the determination of cadmium in fuel alcohol using solid-phase extraction with a flow injection analysis system and detection by flame atomic absorption spectrometry was developed. The sorbent material used was a vermicompost commonly used as a garden fertilizer. The chemical and flow variables of the on-line preconcentration system were optimized by means of a full factorial design. The selected factors were: sorbent mass, sample pH, buffer concentration and sample flow rate. The optimum extraction conditions were obtained using sample pH in the range of 7.3-8.3 buffered with tris(hydroxymethyl)aminomethane at 50 mmol L⁻¹, a sample flow rate of 4.5 mL min⁻¹ and 160 mg of sorbent mass. With the optimized conditions, the preconcentration factor, limit of detection and sample throughput were estimated as 32 (for preconcentration of 10 mL sample), 1.7 μg L⁻¹ and 20 samples per hour, respectively. The analytical curve was linear from 5 up to at least 50 μg L⁻¹, with a correlation coefficient of 0.998 and a relative standard deviation of 2.4% (35 μg L⁻¹, n = 7). The developed method was successfully applied to spiked fuel alcohol, and accuracy was assessed through recovery tests, with recovery ranging from 94% to 100%.     

On-line solid phase extraction system using 1,10-phenanthroline immobilized on surfactant coated alumina for the flame atomic absorption spectrometric determination of copper and cadmium

An on-line solid phase extraction (SPE) preconcentration system coupled to flame atomic absorption spectrometer (FAAS) was developed for determination of copper and cadmium at μg L⁻¹ level. The method is based on the on-line retention of copper and cadmium on a microcolumn of alumina modified with sodium dodecyl sulfate (SDS) and 1,10-phenanthroline and subsequent elution with ethanol and determination by FAAS. The effect of chemical and flow variables that could affect the performance of the system was investigated. The relative standard deviation (n = 6) at 20 μg L⁻¹ level for copper and cadmium were 1.4 and 2.2% and the corresponding limits of detection (based on 3σ) were 0.04 and 0.14 μg L⁻¹, respectively. The method was successfully applied to determination of copper and cadmium in human hair and water samples.     

Determination of cadmium with a sequential injection lab-on-valve by anodic stripping voltammetry using a nafion coated bismuth film electrode

This work exploited a sequential injection lab-on-valve (LOV) system for the determination of cadmium by anodic stripping voltammetry (ASV). A miniaturized electrochemical flow cell (EFC) was fabricated in LOV, in which a nafion coated bismuth film electrode was used as working electrode. The cadmium was electrodeposited on the electrode surface in bismuth solution, and measured with the subsequential stripping scan. Under optimal conditions, the proposed system responded linearly to cadmium concentrations in a range 2.0-100.0 μg L⁻¹. The detection limit of this method was found to be 0.88 μg L⁻¹. By loading a sample volume of 800 μL, a sampling frequency of 22 determinations h⁻¹ was achieved. The repeatability expressed as relative standard derivation (R.S.D.) was 3.65% for 20 μg L⁻¹ cadmium (n = 11). The established method was applied to analysis of trace cadmium in environmental water samples and the spiked recoveries were satisfactory.     

Development of a flow system for the determination of low concentrations of silver using Moringa oleifera seeds as biosorbent and flame atomic absorption spectrometry

In this study a method for the determination of low concentrations of silver in waters using solid-phase extraction with a flow injection analysis system and detection by flame atomic absorption spectrometry (FAAS) was developed. Moringa oleifera seeds were used as a biosorbent material. Chemical and flow variables of the on-line preconcentration system such as sample pH and flow rate, preconcentration time, eluent concentration and sorbent mass were studied. The optimum preconcentration conditions were obtained using sample pH in the range of 6.0-8.0, preconcentration time of 4 min at a flow rate of 3.5 mL min^− 1, 0.5 mol L^− 1 HNO₃ eluent at a flow rate of 4.5 mL min^− 1 and 35 mg of sorbent mass. With the optimized conditions, the preconcentration factor, precision, detection limit and sample throughput were estimated as 35 (for preconcentration of 14 mL sample), 3.8% (5.0 μg L^− 1, n = 7), 0.22 μg L^− 1 and 12 samples per hour, respectively. The developed method was successfully applied to mineral water and tap water, and accuracy was assessed through analysis of a certified reference material for water (APS-1071 NIST) and recovery tests, with recovery ranging from 94 to 101%.     

Determination of cadmium, lead and thallium in highly saline hemodialysis solutions by potentiometric stripping analysis (PSA)

Potentiometric stripping analysis (PSA) was investigated to assay simultaneously cadmium, lead and thallium present as contaminants in highly saline solutions used in hemodialysis. The saline matrices were sodium, potassium, magnesium and calcium chlorides, sodium acetate, sodium bicarbonate and glucose, which constitute concentrates for hemodialysis. A 1000 μg mL⁻¹ Hg(II) solution was used to prepare the mercury film electrode (MFE) and to carry out the stripping step. After a 30 s accumulation interval the analytes were simultaneously detected in the saline matrices without using masking agents. Determination limits of 80 ng L⁻¹ for cadmium and thallium, and 50 ng L⁻¹ for lead were calculated and a R.S.D. ranging from 0.5 to 2.2% (n = 3) was obtained measuring the analytes directly in commercial hemodialysis saline solutions. Recoveries from spiked samples ranging from 94.6 to 102.0% were obtained. The investigated metals were found in concentrations ranging from 2.7 to 5.7 μg L⁻¹ for cadmium, 27.7 to 75.8 μ L⁻¹ for lead and 9.6 to 18.7 μg L⁻¹ for thallium in commercial hemodialysis solutions. The PSA method showed to be adequate to the quality control of saline concentrates for hemodialysis.     

The use of a polymer inclusion membrane for separation and preconcentration of orthophosphate in flow analysis

A highly sensitive flow analysis system has been developed for the trace determination of reactive phosphate in natural waters, which uses a polymer inclusion membrane (PIM) with Aliquat 336 as the carrier for on-line analyte separation and preconcentration. The system operates under flow injection (FI) and continuous flow (CF) conditions. Under optimal FI conditions the system is characterised by a linear concentration range between 0.5 and 1000 μg L⁻¹ P, a sampling rate of 10 h⁻¹, a limit of detection of 0.5 μg L⁻¹ P and RSDs of 3.2% (n = 10, 100 μg L⁻¹) and 7.7% (n = 10, 10 μg L⁻¹). Under CF conditions with 10 min stop-flow time and sample solution flow rate of 1.32 mL min⁻¹ the flow system offers a limit of detection of 0.04 μg L⁻¹ P, a sampling rate of 5 h⁻¹ and an RSD of 3.4% (n = 5, 2.0 μg L⁻¹). Interference studies revealed that anions commonly found in natural waters did not interfere when in excess of at least one order of magnitude. The flow system, operating under CF conditions, was successfully applied to the analysis of natural water samples containing concentrations of phosphate in the low μg L⁻¹ P range, using the multipoint standard addition method.     

Simple hollow fiber renewal liquid membrane extraction method for pre-concentration of Cd(II) in environmental samples and detection by Flame Atomic Absorption Spectrometry

A hollow fiber renewal liquid membrane (HFRLM) extraction method to determine cadmium (II) in water samples using Flame Atomic Absorption Spectrometry (FAAS) was developed. Ammonium O,O-diethyl dithiophosphate (DDTP) was used to complex cadmium (II) in an acid medium to obtain a neutral hydrophobic complex (ML₂). The organic solvent introduced to the sample extracts this complex from the aqueous solution and carries it over the poly(dimethylsiloxane) (PDMS) membrane, that had their walls previously filled with the same organic solvent. The organic solvent is solubilized inside the PDMS membrane, leading to a homogeneous phase. The complex strips the lumen of the membrane where, at higher pH, the complex Cd-DDTP is broken down and cadmium (II) is released into the stripping phase. EDTA was used to complex the cadmium (II), helping to trap the analyte in the stripping phase. A multivariate procedure was used to optimize the studied variables. The optimized variables were: sample (donor phase) pH 3.25, DDTP concentration 0.05% (m/v), stripping (acceptor phase) pH 8.75, EDTA concentration 1.5 × 10⁻² mol L⁻¹, extraction temperature 40 °C, extraction time 40 min, a solvent mixture N-butyl acetate and hexane (60/40%, v/v) with a volume of 100 μL, and addition of ammonium sulfate to saturate the sample. The sample volume used was 20 mL and the stripping volume was 165 μL. The analyte enrichment factor was 120, limit of detection (LOD) 1.3 μg L⁻¹, relative standard deviation (RSD) 5.5% and the working linear range 2-30 μg L⁻¹.     

On-line sorptive preconcentration platform incorporating a readily exchangeable Oasis HLB extraction micro-cartridge for trace cadmium and lead determination by flow injection-flame atomic absorption spectrometry

A simple, sensitive and inexpensive flow injection solid phase extraction (SPE) system was developed for automatic determination of trace level concentrations of metals. The potentials of this novel scheme, coupled to flame atomic absorption spectrometry (FAAS), were demonstrated for trace cadmium and lead determination in environmental water samples. The method was based on on-line chelate complex formation of target species with ammonium diethyldithiophosphate (DDTP), retention onto the surface of reversed-phase poly(divinylbenzene-N-vinylpyrrolidone) co-polymeric beads (Oasis HLB) and elution with methanol prior to atomization. A special PVC adapter was designed for easy and rapid replacement of the commercially available SPE cartridge. All main chemical and hydrodynamic parameters affecting the complex formation, sorption and elution of the analyte were optimized thoroughly. Moreover, the effect of potential interfering species occurring in environmental samples was also explored.For 90 s preconcentration time, enhancement factors of 155 and 180, detection limits (3s) of 0.09 μg L^− 1 and 0.9 μg L^− 1 and relative standard deviations (R.S.D.) of 2.9% (at 4.0 μg L^− 1) and 2.6% (at 20.0 μg L^− 1) were obtained for cadmium and lead, respectively, with a sample throughput of 24 h^− 1. The measurement trueness of the developed method was evaluated by analyzing a certified reference material and spiked environmental water samples. The proposed method is well suited to detect the target elements at concentration levels below the maximum allowed concentrations endorsed by the European Framework Directive (2008/105/EC) in inland and coastal waters.     

Sensitive determination of hydrazine in water by gas chromatography–mass spectrometry after derivatization with ortho-phthalaldehyde

A gas chromatography–mass spectrometric (GC–MS) method has been established for the determination of hydrazine in drinking water and surface water. This method is based on the derivatization of hydrazine with ortho-phthalaldehyde (OPA) in water. The following optimum reaction conditions were established: reagent dosage, 40 mg mL⁻¹ of OPA; pH 2; reaction for 20 min at 70 °C. The organic derivative was extracted with methylene chloride and then measured by GC–MS. Under the established condition, the detection and the quantification limits were 0.002 μg L⁻¹ and 0.007 μg L⁻¹ by using 5.0-mL of surface water or drinking water, respectively. The calibration curve showed good linearity with r² = 0.9991 (for working range of 0.05–100 μg L⁻¹) and the accuracy was in a range of 95–106%, and the precision of the assay was less than 13% in water. Hydrazine was detected in a concentration range of 0.05–0.14 μg L⁻¹ in 2 samples of 10 raw drinking water samples and in a concentration range of 0.09–0.55 μg L⁻¹ in 4 samples of 10 treated drinking water samples.     

Flow injection wetting-film extraction system for flame atomic absorption spectrometric determination of cadmium in environmental waters

A newly simple flow injection wetting-film extraction system coupled to flame atomic absorption spectrometry (FAAS) has been developed for trace amount of cadmium determination. The sample was mixed on-line with sodium diethyl dithiocarbamate and the produced non-charged Cd(II)-diethyl dithiocarbamate (DDTC) chelate complex was extracted on the thin film of diisobutyl ketone (DIBK) on the inner wall of the PTFE extraction coil. The wetting-film with the extracted analyte was then eluted by a segment of the cover solvent, and transported directly to the FAAS for evaluation. All the important chemical and flow parameters were optimized. Under the optimized conditions an enhancement factor of 35, a sample frequency of 22 h⁻¹ and a detection limit of c_L = 0.7 μg l⁻¹ Cd(II) were obtained for 60 s preconcentration time. The calibration curve was linear over the concentration range 1.5-45.0 μg l⁻¹ Cd(II) and the relative standard deviation, R.S.D. (n = 10) was 3.9%, at 10.0 μg l⁻¹ concentration level. The developed method was successfully applied to cadmium determination in a variety of environmental water samples as well as waste-water sample.     

A new flow injection preconcentration method based on multiwalled carbon nanotubes for the ETA-AAS determination of Cd in urine

A new flow injection (FIA) procedure for the preconcentration of cadmium in urine using multiwalled carbon nanotubes (MWCNT) as sorbent and posterior electrothermal atomization atomic absorption spectrometry (ETA-AAS) Cd determination has been developed. Cadmium was retained in a column filled with previously oxidized MWCNTs and it was quantitatively eluted with a nitric acid solution. The parameters influencing the adsorption-elution process such as pH of the sample solution, amount of sorbent and flow rates of sample as well as eluent solutions have been studied. Cd concentration in the eluent was measured by ETA-AAS under the optimized conditions obtained. The results indicated the elimination of urine matrix effect as a consequence of the preconcentration process performed. Total recovery of cadmium from urine at pH 7.2 using a column with 45 mg of MWCNTs as sorbent and employing a HNO₃ 0.5 mol L⁻¹ solution for elution was attained. The detection limit obtained was 0.010 μg L⁻¹ and the preconcentration factor achieved was 3.4. The method showed adequate precision (RSD: 3.4-9.8%) and accuracy (mean recovery: 97.4-100%). The developed method was applied for the determination of cadmium in real urine samples from healthy people (in the range of 0.14-2.94 μg L⁻¹) with satisfactory results.     

On-site fuel electroanalysis: Determination of lead,copper and mercury in fuel bioethanol by anodic stripping voltammetry using screen-printed gold electrodes

The potential application of commercial screen-printed gold electrodes (SPGEs) for the trace determination of lead, copper, and mercury in fuel bioethanol is demonstrated. Samples were simply diluted in 0.067 mol L⁻¹ HCl solution prior to square-wave anodic stripping voltammetry (SWASV) measurements recorded with a portable potentiostat. The proposed method presented a low detection limit (<2 μg L⁻¹) for a 240 s deposition time, linear range between 5 and 300 μg L⁻¹, and adequate recovery values (96–104%) for spiked samples. This analytical method shows great promise for on-site trace metal determination in fuel bioethanol once there is no requirement for sample treatment or electrode modification.     

Evaluation of polychlorotrifluoroethylene as sorbent material for on-line solid phase extraction systems: determination of copper and lead by flame atomic absorption spectrometry in water samples

Polychlorotrifluoroethylene (PCTFE) in the form of beads was applied, as packing material for flow injection on-line column preconcentration and separation systems coupled with flame atomic absorption spectrometry (FAAS). Its performance characteristics were evaluated for trace copper determination in environmental samples. The on-line formed complex of metal with diethyldithiophosphate (DDPA) was sorbed on the PCTFE surface. Isobutyl methyl ketone (IBMK) at a flow rate of 2.8 mL min⁻¹ was used to elute the analyte complex directly into the nebulizer-burner system of spectrophotometer. The proposed sorbent material reveal, excellent chemical and mechanical resistance, fast adsorption kinetics permitting the use of high sample flow rates up to 15 mL min⁻¹ without loss of retention efficiency. For copper determination, with 90 s preconcentration time the sample frequency was 30 h⁻¹, the enhancement factor was 250, which could be further improved by increasing the loading (preconcentration) time. The detection limit (3s) was c_L = 0.07 μg L⁻¹, and the precision (R.S.D.) was 1.8%, at the 2.0 μg L⁻¹ Cu(II) level. For lead determination, the detection limit was c_L = 2.7 μg L⁻¹, and the precision (R.S.D.) 2.2%, at the 40.0 μg L⁻¹ Pb(II) level. The accuracy of the developed method was evaluated by analyzing certified reference materials and by recovery measurements on spiked natural water samples.     

Sequential injection anodic stripping voltammetry with monosegmented flow and in-line UV digestion for determination of Zn(II), Cd(II), Pb(II) and Cu(II) in water samples

A cost-effective sequential injection system incorporating with an in-line UV digestion for breakdown of organic matter prior to voltammetric determination of Zn(II), Cd(II), Pb(II) and Cu(II) by anodic stripping voltammetry (ASV) on a hanging mercury drop electrode (HMDE) of a small scale voltammetric cell was developed. A low-cost small scale voltammetric cell was fabricated from disposable pipet tip and microcentrifuge tube with volume of about 3 mL for conveniently incorporated with the SI system. A home-made UV digestion unit was fabricated employing a small size and low wattage UV lamps and flow reactor made from PTFE tubing coiled around the UV lamp. An in-line single standard calibration or a standard addition procedure was developed employing a monosegmented flow technique. Performance of the proposed system was tested for in-line digestion of model water samples containing metal ions and some organic ligands such as strong organic ligand (EDTA) or intermediate organic ligand (humic acid). The wet acid digestion method (USEPA 3010a) was used as a standard digestion method for comparison. Under the optimum conditions, with deposition time of 180 s, linear calibration graphs in range of 10-300 μg L⁻¹ Zn(II), 5-200 μg L⁻¹ Cd(II), 10-200 μg L⁻¹ Pb(II), 20-400 μg L⁻¹ Cu(II) were obtained with detection limit of 3.6, 0.1, 0.7 and 4.3 μg L⁻¹, respectively. Relative standard deviation were 4.2, 2.6, 3.1 and 4.7% for seven replicate analyses of 27 μg L⁻¹ Zn(II), 13 μg L⁻¹ Cd(II), 13 μg L⁻¹ Pb(II) and 27 μg L⁻¹ Cu(II), respectively. The system was validated by certified reference material of trace metals in natural water (SRM 1640 NIST). The developed system was successfully applied for speciation of Cd(II) Pb(II) and Cu(II) in ground water samples collected from nearby zinc mining area.     

Cell-sorption of paramagnetic metal ions on a cell-immobilized micro-column in the presence of an external magnetic field

The cell-sorption of paramagnetic ions of Mn²⁺ and Cr³⁺ onto a Chlorella vulgaris(C. vulgaris) cell-immobilized micro-column was significantly improved in the presence of an external magnetic field generated in a finite solenoid, by placing the micro-column in the center of the solenoid in a sequential injection system. Magnetic field creates an opposite drift velocity on the hydrated paramagnetic ions against the flow of the sample zone, retards the moving velocity of the metal ions and provides extra contacting time with the cells on the micro-column and offers more chances for the paramagnetic ions to interact with the various functional groups or binding sites on the cell surface, which significantly facilitates cell-sorption of the paramagnetic ions. The sorption efficiencies of Mn²⁺ and Cr³⁺ at the 20 μg L⁻¹ level were improved from 45 to 80% and 60 to 90%, respectively, in a magnetic field of 240 mT.The system was applied for the separation/preconcentration of ultra-trace level of manganese. The presence of an external magnetic field significantly alleviated the interfering effects from coexisting metal ions. Within a liner range of 0.025-0.5 μg L⁻¹ and a sampling volume of 500 μL, an enrichment factor of 21.2, a limit of detection of 0.008 μg L⁻¹, along with a sampling frequency of 20 h⁻¹ was attained, achieving a precision of 2.1% R.S.D. (0.2 μg L⁻¹). Manganese contents in a certified reference material of riverine water and a snow water were analyzed.     

Determination of trace heavy metals in herbs by sequential injection analysis-anodic stripping voltammetry using screen-printed carbon nanotubes electrodes

A method for the simultaneous determination of Pb(II), Cd(II), and Zn(II) at low μg L⁻¹ concentration levels by sequential injection analysis-anodic stripping voltammetry (SIA-ASV) using screen-printed carbon nanotubes electrodes (SPCNTE) was developed. A bismuth film was prepared by in situ plating of bismuth on the screen-printed carbon nanotubes electrode. Operational parameters such as ratio of carbon nanotubes to carbon ink, bismuth concentration, deposition time and flow rate during preconcentration step were optimized. Under the optimal conditions, the linear ranges were found to be 2-100 μg L⁻¹ for Pb(II) and Cd(II), and 12-100 μg L⁻¹ for Zn(II). The limits of detection (S_bl/S = 3) were 0.2 μg L⁻¹ for Pb(II), 0.8 μg L⁻¹ for Cd(II) and 11 μg L⁻¹ for Zn(II). The measurement frequency was found to be 10-15 stripping cycle h⁻¹. The present method offers high sensitivity and high throughput for on-line monitoring of trace heavy metals. The practical utility of our method was also demonstrated with the determination of Pb(II), Cd(II), and Zn(II) by spiking procedure in herb samples. Our methodology produced results that were correlated with ICP-AES data. Therefore, we propose a method that can be used for the automatic and sensitive evaluation of heavy metals contaminated in herb items.     

Determination of quinolizidine alkaloids in Sophora medicinal plants by capillary electrophoresis

A new capillary electrophoresis (CE) method for the determination of quinolizidine alkaloids in Sophora medicinal plants was developed. A total of seven alkaloid components (cytisine, sophocarpine, matrine, lehmannine, sophoranol, oxymatrine and oxysophocarpine) were separated within 15 min. The running buffer was a 50 mM phosphate buffer containing 1%HP-β-CD and 3.3% isopropanol. The linear calibration ranges were 5.50-88.0 μg ml⁻¹ for cytisine and lehmannine, 5.00-88.0 μg ml⁻¹ for sophocarpine and sophoranol, 5.60-89.6 μg ml⁻¹ for matrine and oxysophocarpine, and 24.0-384 μg ml⁻¹ for oxymatrine. The recoveries of the seven alkaloids were 96.0-102.9% with relative standard deviations from 1.50 to 3.00% (n = 5). The method was successfully applied to different Sophora medicinal plants including Sophora flavescens, Sophora tonkinensis and Sophora alopecuroides.     

Use of Nb(2)O(5)-SiO(2) in an automated on-line preconcentration system for determination of copper and cadmium by FAAS

A procedure for the determination of trace level of copper(II) and cadmium(II) by FAAS using an on-line preconcentration system has been proposed. In this system, copper and cadmium ions were adsorbed onto a minicolumn packed with silica gel modified with niobium(V) oxide (Nb₂O₅-SiO₂), followed by nitric acid elution in reverse mode and determination on-line by flame atomic absorption spectrometry (AAS) without interference of the matrix. Chemical and flow variables as well as concomitant ions were studied in the developed procedure. The enrichment factor for copper(II) and cadmium(II) was 34.2 and 33.0, respectively, using a preconcentration time of 2 min. The limit of detection for copper(II) and cadmium(II) was 0.4, and 0.1 μg l⁻¹, respectively. The precision of the method, evaluated as the relative standard deviation in solutions containing 15 μg l⁻¹ of copper and 10 μg l⁻¹ of cadmium, by analyzing a series of seven replicates, was 1.8 and 1.6%, respectively. The accuracy was assessed through recovery experiments of certified material and water samples.     

Synthesis of three haptens for the class-specific immunoassay of O,O-dimethyl organophosphorus pesticides and effect of hapten heterology on immunoassay sensitivity

A general and broad class-specific enzyme-linked immunosorbent assay was developed for the O,O-dimethyl organophosphorus pesticides, including malathion, dimethoate, phenthoate, phosmet, methidathion, fenitrothion, methyl parathion and fenthion. Three haptens with different spacer-arms were synthesized. The haptens were conjugated to bovine serum albumin (BSA) for immunogens and to ovalbumin (OVA) for coating antigens. Rabbits were immunized with the immunogens and six polyclonal antisera were produced and screened against each of the coating antigens using competitive indirect enzyme-linked immunosorbent assay for selecting the proper antiserum. The effect of hapten heterology on immunoassay sensitivity was also studied. The antibody-antigen combination with the most selectivity for malathion was further optimized and tested for tolerance to co-solvent, pH and ionic strength changes. The IC₅₀ values, under optimum conditions, were estimated to be 30.1 μg L⁻¹for malathion, 28.9 μg L⁻¹ for dimethoate, 88.3 μg L⁻¹ for phenthoate, 159.7 μg L⁻¹ for phosmet, 191.7 μg L⁻¹ for methidathion, 324.0 μg L⁻¹ for fenitrothion, 483.9 μg L⁻¹ for methyl parathion, and 788.9 μg L⁻¹ for fenthion. Recoveries of malathion, dimethoate, phenthoate, phosmet and methidathion from fortified Chinese cabbage samples ranged between 77.1% and 104.7%. This assay can be used in monitoring studies for the multi-residue determination of O,O-dimethyl organophosphorus pesticides.     

Determination of trace bisphenol A in complex samples using selective molecularly imprinted solid-phase extraction coupled with capillary electrophoresis

The highly selective, fast and effective sample pretreatment technique molecularly imprinted solid-phase extraction (MISPE) can overcome the low sensitivity of the highly efficient capillary electrophoresis-UV method (CE-UV). In this work, narrowly dispersible bisphenol A (BPA)-imprinted polymeric microspheres with a high capacity factor of k′ = 6.8 and an imprinted factor of I = 6.53 were investigated as selective solid-phase extraction (SPE) sorbents for use in extraction of BPA from different sample matrices (tap water, wastewater, Yangtze River water, soil from the Yangtze River, shrimp and human urine). Washing and eluting protocols of MISPE were optimized. Under optimal conditions, recoveries of MISPE were investigated. Recoveries were basically constant and the relative standard deviation (RSD) was lower than 5.8% when loading volumes changed from 1 to 50 mL. Recoveries ranged from 71.20% to 86.23% for different sample matrices. Compared with C18 SPE, MISPE had higher selectivity and recovery for BPA. BPA was determined with good accuracy and precision in different complex samples using CE-UV coupled with MISPE. Spiked recoveries ranged from 95.20% to 105.40%, and the RSD was less than 7.2%. Because a large loading volume was achieved, the enrichment efficiency of pretreatment and the sensitivity of this method were improved. The limits of detection of this MISPE-CE-UV method for BPA in tap water, wastewater, Yangtze River water, soil from the Yangtze River, shrimp and human urine were 3.0 μg L^− 1, 5.4 μg L^− 1, 6.9 μg L^− 1, 2.1 μg L^− 1, 1.8 μg L^− 1 and 84 μg L^− 1, respectively.