凝固漂浮有机液滴-分散液液微萃取结合高效液相色谱法同时测定地表水中多环芳烃和酞酸酯

多环芳烃和酞酸酯是国际公认的优控污染物,因此准确快速地测定水中多环芳烃和酞酸酯非常重要。凝固漂浮有机液滴-分散液液微萃取(DLLME-SFO)是一种简便、快速、环境友好、灵敏度高的样品前处理技术。采用DLLME-SFO同时测定地表水中多环芳烃和酞酸酯的分析方法鲜有报道。该文采用凝固漂浮有机液滴-分散液液微萃取富集技术,结合高效液相色谱紫外/荧光法,建立了同时测定地表水中16种多环芳烃和6种酞酸酯的分析方法。考察优化了影响萃取效率的主要因素,包括萃取剂的种类和用量、分散剂的种类和用量、萃取时间和离子强度等。优化后的萃取实验条件为:5.0 mL水样,10μL十二醇为萃取溶剂,500μL甲醇为分散溶剂,涡旋振荡时间2 min,氯化钠用量0.2 g。目标化合物经多环芳烃专用色谱柱(SUPELCOSIL^TM LC-PAH, 150 mm×4.6 mm, 5μm)结合乙腈-水梯度洗脱分离,16种多环芳烃除苊烯外采用荧光检测,苊烯和6种酞酸酯采用紫外检测,外标法定量。结果表明,22种目标化合物的基质加标回收率为60.2%～113.5%,相对标准偏差为1.9%～14.3%;多环芳...     

漂浮液滴固化分散液液微萃取与高效液相色谱联用检测环境水样中的3种烷基苯酚

建立了漂浮液滴固化分散液液微萃取(DLLME-SFO)方法,以脂肪酸作为萃取剂,以甲醇作为分散剂,与高效液相色谱联用检测了环境水样中3种烷基苯酚。对影响前处理方法的因素进行了详细考察,在最佳萃取条件(60μL萃取剂辛酸、600μL分散剂甲醇、pH值为2.0~8.0、10 mL水样中加入0.5 g NaCl)下,3种烷基苯酚在20~1 500μg/L范围内具有良好的线性关系,相关系数不小于0.998 5,3种目标化合物的检出限为0.45~0.61μg/L,富集倍数为145~169,实际样品中3个水平的加标回收率为80.1%~109.9%。该方法将脂肪酸作为萃取剂,与HPLC联用实现了烷基苯酚的富集与检测,为环境水样中烷基苯酚的检测提供了对环境友好的前处理新方法。     

Centrifugeless ultrasound‐assisted emulsification microextraction based on salting‐out phenomenon followed by high‐performance liquid chromatography for the simple determination of phthalate esters in aqueous samples

A fast, sensitive, and centrifugeless ultrasound‐assisted emulsification microextraction followed by a high‐performance liquid chromatography method is developed for the determination of some phthalate esters in aqueous samples. In this method, a simple approach is followed to eliminate the centrifugation step in dispersive liquid–liquid microextraction using an organic solvent whose melting point is near the ambient temperature, consumption of the extracting solvent is efficiently reduced, and the overall extraction time was found to be only 7 min. The variables affecting the method are optimized. Under the optimal experimental conditions (75 μL of 1‐undecanol, a flow rate of 2.0 mL/min, and an ultrasound irradiation of 1 min), the proposed method exhibits good preconcentration factors (52–97), low limits of detection (1.0–5.0 ng/mL), and linearities in the range of 5–1500 ng/mL (r ² ≥ 0.995). Finally, the method is successfully applied to the analysis of phthalate esters in the drinking and river water samples. To study the probable release of the phthalate esters from a polyethylene container into boiling water, the boiling water exposed to the polyethylene container was analyzed by the proposed method.     

A novel dispersive liquid-liquid microextraction based on solidification of floating organic droplet method for determination of polycyclic aromatic hydrocarbons in aqueous samples

A new dispersive liquid-liquid microextraction based on solidification of floating organic droplet method (DLLME-SFO) was developed for the determination of five kinds of polycyclic aromatic hydrocarbons (PAHs) in environmental water samples. In this method, no specific holder, such as the needle tip of microsyringe and the hollow fiber, is required for supporting the organic microdrop due to the using of organic solvent with low density and proper melting point. Furthermore, the extractant droplet can be collected easily by solidifying it in the lower temperature. 1-Dodecanol was chosen as extraction solvent in this work. A series of parameters that influence extraction were investigated systematically. Under optimal conditions, enrichment factors (EFs) for PAHs were in the range of 88-118. The limit of detections (LODs) for naphthalene, diphenyl, acenaphthene, anthracene and fluoranthene were 0.045, 0.86, 0.071, 1.1 and 0.66 ng mL⁻¹, respectively. Good reproducibility and recovery of the method were also obtained. Compared with the traditional liquid-phase microextraction (LPME) and dispersive liquid-liquid microextraction (DLLME) methods, the proposed method obtained about 2 times higher enrichment factor than those in LPME. Moreover, the solidification of floating organic solvent facilitated the phase transfer. And most importantly, it avoided using high-density and toxic solvent in the traditional DLLME method. The proposed method was successfully applied to determinate PAHs in the environmental water samples. The simple and low-cost method provides an alternative method for the analysis of non-polar compounds in complex environmental water.     

悬浮固化分散液液微萃取-高效液相色谱法测定水体中邻苯二甲酸酯

建立了悬浮固化分散液液微萃取（SFO-DLLME）结合高效液相色谱（HPLC）快速测定水样中6种邻苯二甲酸酯（PAEs）的分析方法。通过对影响萃取效率因素的优化,确定了最佳萃取条件：十二烷醇萃取剂20 μL、萃取温度60℃、离子强度20 g/L、萃取时间1 min。6种PAEs在2~2000 μg/L范围内呈良好的线性关系,相关系数（r）为0.9995~0.9999,检出限（S/N=3）为0.3~0.6 μg/L。对自来水、湖水、江水、污水、海水、市售塑料瓶装纯净水和矿泉水进行测定,能检测到部分PAEs。对加标水样进行回收率试验（10、100和1000 μg/L）,6种PAEs的回收率为84.9%~94.5%,相对标准偏差为4.1%~6.8%（n=5）。该法环保、简单,可用于实际水样中6种PAEs的检测分析。     

Ultrasound-assisted surfactant-enhanced emulsification microextraction for the determination of carbamate pesticides in water samples by high performance liquid chromatography

A novel ultrasound-assisted surfactant-enhanced emulsification microextraction (UASEME) coupled with high performance liquid chromatography-diode array detection has been developed for the extraction and determination of six carbamate pesticides (metolcarb, carbofuran, carbaryl, pirimicarb, isoprocarb and diethofencarb) in water samples. In the UASEME technique, Tween 20 was used as emulsifier, and chlorobenzene and chloroform were used as dual extraction solvent without using any organic dispersive solvent that is normally required in the previously described common dispersive liquid–liquid microextraction method. Parameters that affect the extraction efficiency, such as the kind and volume of the extraction solvent, the type and concentration of the surfactant, ultrasound emulsification time and salt addition, were investigated and optimized for the method. Under the optimum conditions, the enrichment factors were in the range between 170 and 246. The limits of detection of the method were 0.1–0.3 ng mL⁻¹ and the limits of quantification were between 0.3 and 0.9 ng mL⁻¹, depending on the compounds. The linearity of the method was obtained in the range of 0.3–200 ng mL⁻¹ for metolcarb, carbaryl, pirimicarb, and diethofencarb, 0.6–200 ng mL⁻¹ for carbofuran, and 0.9–200 ng mL⁻¹ for isoprocarb, with the correlation coefficients (r) ranging from 0.9982 to 0.9998. The relative standard deviations varied from 3.2 to 4.8% (n = 5). The recoveries of the method for the six carbamates from water samples at spiking levels of 1.0, 10.0, 50.0 and 100.0 ng mL⁻¹ were ranged from 81.0 to 97.5%. The proposed UASEME technique has demonstrated to be simple, practical and environmentally friendly for the determination of carbamates residues in river, reservoir and well water samples.     

Ultrasound-assisted emulsification microextraction method based on applying low density organic solvents followed by gas chromatography analysis for the determination of polycyclic aromatic hydrocarbons in water samples

In this study, a fast, simple and efficient ultrasound-assisted emulsification microextraction (USAEME) method was successfully developed based on applying low density organic solvents. Fourteen microliters of toluene was injected slowly into a 12 mL home-designed centrifuge glass vial containing an aqueous sample that was located inside the ultrasonic water bath. The formed emulsion was centrifuged and 2 μL of separated toluene (about 4 μL) was injected into a gas chromatographic system equipped with a flame ionization detector (GC-FID) for analysis. Some polycyclic aromatic hydrocarbons (PAHs) were selected as model compounds for developing the method and evaluating its performance and to compare the efficiency of the proposed method with previously reported techniques. Several factors influencing the emulsification, extraction and collection efficiency such as the nature and volume of organic solvent, emulsification–extraction temperature, ionic strength and equilibrium and centrifugation times were investigated and optimized. Under the optimum conditions, preconcentration factors (PFs) in a range of 1776–2714 were obtained. The performance of the proposed method was studied in terms of linear dynamic range (LDRs from 0.05 to 100 μg L⁻¹), linearity (R² ≥ 0.994), precision (repeatability: RSD% ≤ 7.9, reproducibility: RSD% ≤ 14.6) and extraction percents (59.2–90.5%). Limits of detection (LODs) in the range of 0.02–0.05 μg L⁻¹ were obtained for different PAHs. The applicability of the proposed method was evaluated by the extraction and determination of PAHs from several natural water samples.     

Determination of volatile organic compounds in water using ultrasound-assisted emulsification microextraction followed by gas chromatography

Volatile organic compounds (VOCs) are toxic compounds in the air, water and land. In the proposed method, ultrasound-assisted emulsification microextraction (USAEME) combined with gas chromatography-mass spectrometry (GC-MS) has been developed for the extraction and determination of eight VOCs in water samples. The influence of each experimental parameter of this method (the type of extraction solvent, volume of extraction solvent, salt addition, sonication time and extraction temperature) was optimized. The procedure for USAEME was as follows: 15 μL of 1-bromooctane was used as the extraction solvent; 10 mL sample solution in a centrifuge tube with a cover was then placed in an ultrasonic water bath for 3 min. After centrifugation, 2 μL of the settled 1-bromooctane extract was injected into the GC-MS for further analysis. The optimized results indicated that the linear range is 0.1-100.0 μg/L and the limits of detection (LODs) are 0.033-0.092 μg/L for the eight analytes. The relative standard deviations (RSD), enrichment factors (EFs) and relative recoveries (RR) of the method when used on lake water samples were 2.8-9.5, 96-284 and 83-110%. The performance of the proposed method was gauged by analyzing samples of tap water, lake water and river water samples.     

Optimization of simultaneous derivatization and extraction of aliphatic amines in water samples with dispersive liquid-liquid microextraction followed by HPLC

Dispersive liquid-liquid microextraction based on solidification of floating organic droplet (DLLME-SFO) with simultaneous derivatization followed by high-performance liquid chromatography-diode array detection (HPLC-DAD) was applied for preconcentration and determination of primary and secondary aliphatic amines in environmental water samples. A ternary mixture consisting of a disperser, an extractant and a derivatization reagent was used for the simultaneous derivatization and extraction of aliphatic amines in different water samples. The effects of various experimental parameters on derivatization and extraction efficiency were studied simultaneously using experimental design. A Plackett-Burman design was performed for screening of variables in order to determine the significant variables affecting the extraction efficiency. Then, the significant factors were optimized by using a Box-Behnken design (BBD) and the response surface equations were derived. Under optimal conditions, the preconcentration factors were between 210 and 290. The limit of detections (LODs) ranged from 0.005 to 0.02 μg/L and dynamic linear ranges (DLRs) of 0.05-500 and 0.1-500 μg/L were obtained for most of analytes. The performance of the method was evaluated for extraction and determination of primary and secondary aliphatic amines in environmental water samples in micrograms per liter and satisfactory results were obtained (RSDs <12.5%).     

Development of ultrasound-assisted emulsification microextraction for the determination of triazine herbicides in environmental water samples by high-performance liquid chromatography

A simple, rapid, efficient, and environmentally friendly method for the determination of some triazine herbicides (simazine, atrazine, prometone, ametryn and prometryne) in water samples was developed by ultrasound-assisted emulsification microextraction (USAEME) coupled with high-performance liquid chromatography-diode array detection (HPLC-DAD). The main parameters that affect the extraction efficiencies, such as the kind and volume of the extraction solvent, ultrasound emulsification time and salt addition, were investigated and optimized. Under the optimum conditions, the method was sensitive and showed a good linearity within a range of 0.5 to 200?ngm?L^?1 for simazine, atrazine, prometone, ametryn and prometryne, with the correlation coefficients (r) varying from 0.9993 to 0.9998. High enrichment factors were obtained ranging from 148 to 225. The limits of detection (LODs) were in the range between 0.06 and 0.1?ngm?L^?1 and the limits of quantification (LOQs) were in the range between 0.2 and 0.3?ngm?L^?1. The recoveries of the analytes from water samples at spiking levels of 5.0 and 50.0?ngm?L^?1 were ranged from 82.4% to 107.0%. The relative standard deviations (RSDs) varied from 3.0% to 4.6%. The results demonstrated that the USAEME-HPLC-DAD method was an ef?cient pretreatment and enrichment procedure for the determination of triazine pesticides in real water samples.     

Application of dispersive liquid-liquid microextraction and high-performance liquid chromatography for the determination of three phthalate esters in water samples

A novel method, dispersive liquid-liquid microextraction (DLLME) coupled with high-performance liquid chromatography-variable wavelength detector (HPLC-VWD), has been developed for the determination of three phthalate esters (dimethyl phthalate (DMP), diethyl phthalate (DEP), and di-n-butyl phthalate (DnBP)) in water samples. A mixture of extraction solvent (41 μL carbon tetrachloride) and dispersive solvent (0.75 mL acetonitrile) were rapidly injected into 5.0 mL aqueous sample for the formation of cloudy solution, the analytes in the sample were extracted into the fine droplets of CCl₄. After extraction, phase separation was performed by centrifugation and the enriched analytes in the sedimented phase were determined by HPLC-VWD. Some important parameters, such as the kind and volume of extraction solvent and dispersive solvent, extraction time and salt effect were investigated and optimized. Under the optimum extraction condition, the method yields a linear calibration curve in the concentration range from 5 to 5000 ng mL⁻¹ for target analytes. The enrichment factors for DMP, DEP and DnBP were 45, 92 and 196, respectively, and the limits of detection were 1.8, 0.88 and 0.64 ng mL⁻¹, respectively. The relative standard deviations (R.S.D.) for the extraction of 10 ng mL⁻¹ of phthalate esters were in the range of 4.3-5.9% (n = 7). Lake water, tap water and bottled mineral water samples were successfully analyzed using the proposed method.     

Dispersive liquid–liquid microextraction based on solidification of floating organic droplet for the determination of triazine and triazoles in mineral water samples

A simple, rapid, and sensitive method for the determination of atrazine, simazine, cyproconazole, tebuconazole, and epoxiconazole in mineral water employing the dispersive liquid–liquid microextraction with solidification of a floating organic drop with determination by liquid chromatography tandem mass spectrometry has been developed. A mixed solution of 250 μL 1‐dodecanol and 1250 μL methanol was injected rapidly into 10 mL aqueous solution (pH 7.0) with 2% w/v NaCl. After centrifugation for 5 min at 2000 rpm, the organic solvent droplets floated on the surface of the aqueous solution and the floating solvent solidified. The method limits of detection were between 3.75 and 37.5 ng/L and limits of quantification were between 12.5 and 125 ng/L. The recoveries ranged from 70 to 118% for repeatability and between 76 and 95% for intermediate precision with a relative standard deviation from 2 to 18% for all compounds. Low matrix effect was observed. The proposed method can be successfully applied in routine analysis for determination of pesticide residues in mineral water samples, allowing for monitoring of triazine and triazoles at levels below the regulatory limits set by international and national legislations.     

超声辅助分散液液微萃取-高效液相色谱测定水样中的4种邻苯二甲酸酯类增塑剂

建立了采用超声辅助分散液液微萃取技术结合高效液相色谱法(UA-DLLME-HPLC)对4种邻苯二甲酸酯(PAEs)进行富集、检测的方法,并成功应用于实际水样分析。实验中采用富集因子来评价萃取效率,考察并优化了影响萃取效率的主要因素,包括萃取剂类型和用量、分散剂类型和用量、超声时间、离子强度、萃取时间和pH值等。结果表明: 在最佳萃取条件下,该法对4种PAEs（邻苯二甲酸二甲酯、邻苯二甲酸二乙酯、邻苯二甲酸二丁酯和邻苯二甲酸二正辛酯）具有较高的富集能力,富集因子分别为71、144、169和159;检出限分别为3.78、1.77、3.07和3.30 μg/L。对实验室自来水、某品牌矿泉水以及湖水分别加标50、200及500 μg/L的回收率为82.99%～114.47%,相对标准偏差为1.93%～8.31%。该法简便、快速、环保,可以用于测定实际水样中的PAEs类增塑剂。     

A novel liquid-phase microextraction method combined with high performance liquid chromatography for analysis of phthalate esters in landfill leachates

A novel liquid-phase microextraction (LPME) method was presented in this paper. The most attractive feature of this method is using a polychloroprene rubber tube (PCR tube) instead of a microsyringe to load organic solvent. The PCR tube and sample vial were horizontally placed so that the selection of organic solvent was not affected by the density of extractant. Therefore, the stability of organic solvent increased and the available organic solvent was extended greatly. In this work, three phthalate esters (PAEs) (dimethyl phthalate (DMP), diethyl phthalate (DEP), and di-n-butyl phthalate (DnBP)) were chosen as model analytes to testify the feasibility of the new method. A series of extraction parameters have been investigated systematically. Under the optimized condition, the method showed linear response over four orders of magnitude, ranged from 0.005 mg L⁻¹ to 50 mg L⁻¹. The correlation coefficients (r) were better than 0.997 and the limits of detection (LOD) were 0.0012 mg L⁻¹ for DMP, 0.0014 mg L⁻¹ for DEP and 0.0022 mg L⁻¹ for DnBP. Good reproducibility of extraction was acquired, the inter-day and intra-day relative standard deviation (R.S.D.) were below 7.9% and 7.4%, respectively. Recoveries that ranged from 82.7% to 116.9% were gained when the new method was used to determine three phthalate esters in landfill leachates. The enrichment factors were 5–26 for the three PAEs. The novel LPME is promising to be an alternative sample preparation method for extracting target analytes in complex sample matrices because of the simplicity, low cost and short sample preparation time.     

Determination of haloperidol in biological samples with the aid of ultrasound‐assisted emulsification microextraction followed by HPLC‐DAD

A rapid and simple quantitative method for preconcentration and determination of haloperidol in biological samples was developed using ultrasound‐assisted emulsification microextraction, based on the solidification of floating organic droplet combined with HPLC‐DAD. The effects of several factors were investigated. A total of 30 μL of 1‐undecanol as an extraction solvent was injected slowly into a glass‐centrifuge tube containing 4 mL alkaline sample solution that was located inside the ultrasonic water bath. The formed emulsion was centrifuged and the fine droplets of solvent were floated at the top of the test tube, then it was cooled in an ice bath and the solidified solvent was transferred into a conical vial, after melt, the analysis of the extract was carried out by HPLC. Under the optimal conditions, the extraction efficiencies were more than 90% and the preconcentration factors were obtained between 119–122. The LOQs were obtained between 4–8 μg/L and the calibration curves were linear within the range of 4–1000 μg/L. Finally this method was applied to the determination of haloperidol in plasma and urine samples in the range of μg/L and satisfactory results were achieved (RSDs <7%).     

Ultrasound-assisted emulsification microextraction based on solidification of floating organic droplet combined with HPLC-UV for the analysis of antidepressant drugs in biological samples

Ultrasound-assisted emulsification microextraction based on the solidification of floating organic droplet combined with high-performance liquid chromatography-ultra violet (HPLC-UV) detection was applied for the extraction and determination of fluoxetine, citalopram, and venlafaxine as antidepressants drugs in biological samples. In total, 30 μL of undecanol was injected slowly into a glass-centrifuge tube containing 5 mL alkaline sample solution that was located inside the ultrasonic water bath. The formed emulsion was centrifuged and the fine droplets of solvent were floated at the top of the test tube. The test tube was then cooled in an ice bath and the solidified solvent transferred into a conical vial; it melted quickly at room temperature. Then the analysis of the extracts was carried out by high-performance liquid chromatography. Under optimal conditions, the preconcentration factors were between 174 and 316. Detection limits (LODs) of 3 μg/L were obtained and the calibration graphs were linear within the range of 10-1000 μg/L. Finally, the feasibility of the proposed method was successfully confirmed by extraction and determination of the antidepressant drugs in human urine and plasma samples in the range of microgram per liter and suitable results were obtained.     

A novel method for the determination of trace copper in cereals by dispersive liquid-liquid microextraction based on solidification of floating organic drop coupled with flame atomic absorption spectrometry

A novel,simple,rapid,efficient and environment-friendly method for the determination of trace copper in cereal samples was developed by using dispersive liquid-liquid microextraction based on solidification of floating organic drop(DLLME-SFO) followed by flame atomic absorption spectrometry.In the DLLME-SFO,copper was complexed with 8-hydroxy quinoline and extracted into a small volume of 1-dodecanol,which is of low density,low toxicity and proper melting point near room temperature. The experimental parameters affecting the extraction efficiency were investigated and optimized.Under the optimum conditions, the calibration graph exhibited linearity over the range of 0.5—500 ng/mL with the correlation coefficient(r) of 0.9996.The enrichment factor was 122 and the limit of detection was 0.1 ng/mL.The method was applied to the determination of copper in the complex matrix samples such as rice and millet with the recoveries for the spiked samples at 5.0 and 10.0 u,g/g falling in the range of 92.0-98.0%and the relative standard deviation of 3.9-5.7%.     

有机悬浮固化分散液-液微萃取测定水样中痕量铅

建立了以二乙基二硫代氨基甲酸钠为配位剂,十二醇为萃取剂,乙醇为分散剂的悬浮固化分散液-液微萃取—火焰原子吸收光谱法测定水样中痕量铅的方法。详细探讨了影响萃取效率的因素。优化条件为:二乙基二硫代氨基甲酸钠的用量为10-6 mol,十二醇体积为90.00μL,乙醇体积为1.00 mL,pH为7.00。在最佳条件下,铅的检出限为1.12μg/L,富集倍率为16.00,线性范围5.00～600.00μg/L,对含有20.00μg/L和600.00μg/L Pb的标准溶液平行萃取测定11次,测定结果的RSD分别为3.73%和2.62%。本方法应用于自来水、河水及海水中痕量铅的分析,加标回收率为90.10%～100.70%。     

Determination of phthalate esters in water samples by ionic liquid cold-induced aggregation dispersive liquid-liquid microextraction coupled with high-performance liquid chromatography

A novel method, termed ionic liquid cold-induced aggregation dispersive liquid–liquid microextraction (IL-CIA-DLLME), combined with high-performance liquid chromatography (HPLC) was developed for the determination of three phthalate esters in water samples. Several important parameters influencing the IL-CIA-DLLME extraction efficiency, such as the type of extraction and disperser solvent, the volume of extraction and disperser solvent, temperature, extraction time and salt effect, were investigated. Under optimal extraction conditions, the enrichment factors and extraction recoveries ranged from 174 to 212 and 69.9 to 84.8%, respectively. Excellent linearity with coefficients of correlation from 0.9968 to 0.9994 was observed in the concentration range of 2–100 ng mL⁻¹. The repeatability of the proposed method expressed as relative standard deviations ranged from 2.2 to 3.7% (n = 5). Limits of detection were between 0.68 and 1.36 ng mL⁻¹. Good relative recoveries for phthalate esters in tap, bottled mineral and river water samples were obtained in the ranges of 91.5–98.1%, 92.4–99.2% and 90.1–96.8%, respectively. Thus, the proposed method has excellent potential for the determination of phthalate esters in the environmental field.     

Determination of four acidic nonsteroidal anti‐inflammatory drugs in wastewater samples by dispersive liquid–liquid microextraction based on solidification of floating organic droplet and high‐performance liquid chromatography

A simple, environmentally friendly, and sensitive dispersive liquid–liquid microextraction based on solidification of floating organic droplet for the extraction of four acidic nonsteroidal anti‐inflammatory drugs (ketoprofen, naproxen, ibuprofen, and diclofenac) from wastewater samples subsequent by high‐performance liquid chromatography analysis was developed. The influence of extraction parameters such as pH, the effect of solution ionic strength, type of extraction solvent, disperser solvent, and extraction solvent volume were studied. High enrichment factors (283–302) were obtained through the developed method. The method provides good linearity (r > 0.999) in a concentration range of 1–100 μg/L, good intra‐ and inter‐day precision (relative standard deviation < 7%) and low limits of quantification. The relative recoveries of the selected compounds were situated over 80% both in synthetic and real water samples. The developed method has been successfully applied for the analysis of the selected compounds in wastewater samples.