Determination of pyrethroid,organophosphate and organochlorine pesticides in water by headspace solid-phase microextraction

Simultaneous determination of pyrethroid, organophosphate (OP) and organochlorine (OC) pesticides in water was achieved with headspace solid-phase microextraction (HS-SPME) followed by gas chromatography-electron-capture detection (GC-ECD). The parameters affecting HS-SPME of pesticides from water were optimized, including extraction temperature, sample and headspace volumes, and sodium chloride amounts. The effects of desorption temperature, desorption time, and position of the fibre in the GC inlet were also investigated. Extraction temperature was the most important factor affecting the recoveries of analytes, and the optimized temperature was 96°C. The addition of salt did not increase extraction efficiencies of the pesticides from the water. The optimized desorption conditions in the GC were as follows: desorption time of 10?min; desorption temperature of 260°C; and a 2?cm position of the fibre in the inlet. The method detection limits were in the low-ng/L level with a linearity range of 50–1000?ng/L for the OCs, 50–5000?ng/L for the OP, and 50–20?000?ng/L for the pyrethroids. These data demonstrated that HS-SPME is a sensitive method for the determination of pyrethroid, OC, and OP pesticides in water.     

Development and validation of a fully automated online-SPE–ESI–LC–MS/MS multi-residue method for the determination of different classes of pesticides in drinking,ground and surface water

The present work describes a fully automated method based on online solid phase extraction–liquid chromatography–tandem mass spectrometry for the determination of different classes of pesticides, including acidic and polar pesticides and six thiamethoxam metabolites. Sample preconcentration was performed by extracting 4 mL of the sample with a single styrene-divinylbenzene polymer. Elution of the compounds was done within the high performance liquid chromatography gradient and tandem mass spectrometry determination was performed in the selected reaction monitoring mode, by recording 1–3 transitions per compound. The overall pretreatment and analysis time per sample was less than 15 min. Method validation was performed in drinking, ground and surface water. For nearly all compounds a recovery between 70% and 120% could be achieved. The limit of detection ranges from 1.2 to 18 ng/L in drinking water and 3.0 to 23 ng/L in ground and surface water. The correlation coefficients for a calibration range of 0.05–2 µg/L are between 0.9915 and 0.9999. The limit of quantification (LOQ) for all compounds lies below the required limit of 0.1 µg/L, to fulfil the Council Directive 98/83/EC. Most of the compounds easily reach an LOQ below 0.05 µg/L.     

Gas chromatographic–mass spectrometric methodology using solid-phase microextraction for the multiresidue determination of pesticides in surface waters

Solid-phase microextraction (SPME) coupled with gas chromatography–mass spectrometry (GC–MS) and selected ion monitoring (SIM) was used for the analytical determination of priority pesticide residues. Fibers coated with a 65-µm film thickness of polydimethylsiloxane divinylbenzene (PDMS-DVB) were used to extract 31 pesticides of different chemical groups. The quality parameters of the method demonstrated a good precision with detection limits of 1–56?ng/L. Linearity was controlled in the range of 0.1–50?µg/L. The proposed method was applied for the trace-level determination of the target pesticides in surface water samples including three rivers and one lake at the Epirus region (north-west Greece) for a period of one year. The results demonstrate the suitability of the SPME–GC–MS approach for the analysis of multi-residue pesticides in environmental water samples.     

Alkanol-based supramolecular solvent microextraction of organophosphorus pesticides and their determination using high-performance liquid chromatography

A sensitive method for extraction and determination of three organophosphorus pesticides (chlorpyrifos, diazinon, phosalone) using a supramolecular solvent (SUPRAS) made of inverted hexagonal aggregates of alkanol and high-performance liquid chromatography with ultraviolet detection (HPLC–UV) was developed. The studied factors were alkanol amount, THF percentage (v/v), pH and vortex time. According to the full factorial design results, the effective parameters were alkanol amount, THF percentage (v/v) and pH. Then, a CCF was applied to obtain optimal conditions. The optimized conditions were obtained at 100 mg of alkanol, 5% of THF and pH 3.9. The limits of detection of pesticides were 0.5–1.3 ng/mL. The linearity was 1.6–500.0 ng/mL for different pesticides. Relative standard deviations for intra- and inter-day extraction of pesticides were 3.3–5.0 and 5.1–6.3, respectively, for five measurements. The method was also successfully applied for the determination of the pesticides in fruit juice and tap water samples.     

MWCNTs-solid phase extraction combined with ultra-high performance liquid chromatography-tandem mass spectrometry for the determination of eleven organophosphorus pesticides in river water

A method for simultaneous determination of 11 organophosphorus pesticides residues in river water by MWCNTs-solid phase extraction combined with ultra-high performance liquid chromatography/tandem mass spectrometry was developed. After centrifugation and filtration, the target pesticides were enriched with MWCNTs-SPE cartridge. Then the pesticides adsorbed on MWCNTs were eluted with ethyl acetate and dichloromethane, the eluent was dried-up under nitrogen flow and the residue was dissolved in methanol-water (1:1, v/v) as sample solution. The separation was accomplished on a C18 column with the mobile phase consisting of methanol and 0.1% formic acid at 0.20 mL/min in gradient elution. The pesticides were detected in multiple reaction monitoring mode by a triple quadruple mass spectrometer. Good linearities were obtained within 1–200 ng/L, with the correlation coefficients greater than 0.998. The detection and quantification limits were in the ranges of 0.02–1.00 ng/L and 0.07–3.33 ng/L, respectively. The recoveries and relative standard deviations were in the range of 88.3–124.9% and 0.12–20.5%, respectively. The method has been successfully applied to the detection of 34 urban river water samples from Chengdu, China and 7 organophosphorus pesticides were detected with the concentrations of 0.32–211 ng/L.     

固相萃取-气相色谱-质谱联用同时测定河水和海水中87种农药

采用固相萃取-气相色谱-质谱联用技术,建立了河水和海水中87种农药(24种有机磷、15种有机氯、12种唑类、9种拟除虫菊酯类、5种氨基甲酸酯类、7种酰胺类及15种其他新型农药)的多残留同时分析方法。优化了影响分离效果和灵敏度的仪器参数,考察了固相萃取柱柱型及水样体积、pH、盐度的影响,采用NH2柱优化了净化效果,内标法和替代物法用于数据的质量控制。结果表明: 在最佳条件下,各目标农药的方法检出限为0.1～6.6 ng/L;以实际河水和海水为基底,在5 ng/L和20 ng/L的加标水平下,绝大多数目标农药的回收率为60%～120%,相对标准偏差(n=4)为0.01%～9.7%。该法灵敏、准确,已成功地应用于福建九龙江河口区表层水样中多种类农药的复合污染监测,检出包括5种有机磷类、3种酰胺类、4种唑类、3种氨基甲酸酯类、2种拟除虫菊酯类等农药20种。     

Liquid chromatography-tandem mass spectrometry to determine sedative hypnotic drugs in river water and wastewater

A method for simultaneous determination of four benzodiazepines (bromazepam (BMZ), carbamazepine (CBZ), diazepam (DZP) and nordiazepam (NDZ)) and four barbiturates (barbital (BTL), pentobarbital (PTB), phenobarbital (PNB) and secobarbital (SCB)) in river water and wastewater using solid-phase extraction (SPE) followed by liquid chromatography-(electrospray) tandem mass spectrometry (LC-(ESI)MS/MS) was developed. LC-(ESI)MS/MS analysis was performed in positive and negative modes for benzodiazepines and barbiturates, respectively, and in selected reaction monitoring (SRM). Limits of detection (LODs) were in the range of 0.2–5 ng/L for benzodiazepines and 2.5–50 ng/L for barbiturates. Precision (repeatability and reproducibility between days) expressed as %RSD (n = 5) was lower than 17% for low concentration (depending on the matrix between 50 and 250 ng/L for barbiturates, and between 5 and 25 ng/L for benzodiazepines), and lower than 15% for high concentration (between 200 and 1250 ng/L for barbiturates, and between 20 and 125 ng/L for benzodiazepines). Low matrix effect was observed for all compounds, except for BTL (75%) and PTB (–48%) in wastewater. The method was applied to water samples from two sewage treatment plants (STPs) and the rivers Ebre, Ter and Llobregat, located in Catalonia. CBZ was the target compound found at the highest concentration in river water (2.1–3.3 ng/L). In both influent and effluent wastewater samples, PNB, BMZ, CBZ, DZP and NDZ were determined at concentration levels ranging from 5.0 to 2337.3 ng/L.     

Multiresidue fully automated online SPE-HPLC-MS/MS method for the quantification of endocrine-disrupting and pharmaceutical compounds at trace level in surface water

The present work describes the development and validation of a sensitive method for the determination of traces of diverse groups of pharmaceuticals and endocrine disruptors in surface water. Thirty-seven substances have been selected, including 10 pesticides, 6 hormonal steroids and assimilates, 12 pharmaceuticals, 5 alkylphenols, 1 chlorophenol and 3 other well-known human contaminants, 1 UV filter and 2 plasticisers. An automated online solid-phase extraction (SPE) is directly coupled to liquid chromatography–tandem mass spectrometry. Different SPE columns have been tested, and the injection volume has been optimised. The developed analytical methodology is based on the direct injection of 2.5 mL of water sample acidified at pH 1.6 on an Oasis HLB loading column (20 × 2.1 mm) with 5-µm particles. Then, the chromatographic separation is achieved on a Kinetex XB C18 (100 × 2.1 mm; 1.7 µm) column, and the quantification is realised in multiple-reaction monitoring mode. The online SPE step warrants minimal sample handling, low solvent consumption, high sample throughput, saving time and costs. This method allows the quantification of the target analytes in the lower ng/L concentration range, with limits of quantification (LQs) between 100 pg/L and 10 ng/L, 26 compounds having LQ lower than 1 ng/L. The monitoring of two selected MS/MS transitions for each compound allows the reliable confirmation of positive findings even at the LQ level. The developed and validated methodology has been applied to the analysis of various real samples from two French rivers. Twelve target compounds have been detected in the environmental samples, and the major pollutants are pharmaceuticals usually used by humans (paracetamol, carbamazepine, oxazepam, ketoprofen, trimethoprim). The pesticides atrazine and carbendazim have been ubiquitously detected in real samples too. Metronidazole, sulfamethoxazole and diuron were also frequently quantified in the water samples.     

Multiresidue Method for the Determination of Organophosphorus Pesticides in Still Wine and Fortified Wine Using Solid-Phase Microextraction and Gas Chromatography – Tandem Mass Spectrometry

A SPME-GC-MS/MS method for the determination of eight organophosphorus pesticides (azinphos-methyl, chlorpyriphos, chlorpyriphos-methyl, diazinon, fenitrothion, fenthion, malathion, and methidathion) in still and fortified wine was developed. The extraction procedure is simple, solvent free, and without any sample pretreatment. Limits of detection (LOD) and quantitation (LOQ) values in the range 0.1–14.3 µg/L and 0.2–43.3 µg/L, respectively, were obtained. The LOQ values are below the maximum residue levels (MRLs) established by European Regulation for grapes, with the exception of methidathion. Coefficients of correlation (R²) higher than 0.99 were obtained for the majority of the pesticides, in all different wines analyzed.     

Application of dispersive liquid–liquid microextraction with alcoholic solvents followed by HPLC–UV as a sensitive and efficient method for the extraction and determination of citalopram in biological samples using an experimental design

A sensitive and rapid method based on alcoholic-assisted dispersive liquid–liquid microextraction followed by high-performance liquid chromatography for determination of citalopram in human plasma and urine samples was developed. The effects of six parameters (extraction time, stirring speed, pH, volume of extraction and disperser solvents, and ionic strength) on the extraction recovery were investigated and optimized utilizing Plackett–Burman design and Box–Behnken design, respectively. According to Plackett–Burman design results, the volume of disperser solvent, stirring speed, and extraction time had no effect on the recovery of citalopram. The optimized condition was a mixture of 172 µL of 1-octanol as extraction solvent and 400 µL of methanol as disperser solvent, pH of 10.3 and 1% w/v of salt in the sample solution. Replicating the experiment in optimized condition for five times, gave the average extraction recoveries equal to 89.42%. The detection limit of citalopram in human plasma was obtained 4 ng/mL, and the linearity was in the range of 10–1200 ng/mL. The corresponding values for human urine were 5.4 ng/mL with the linearity in the range of 10–2000 ng/mL. Relative standard deviations for inter- and intraday extraction of citalopram were less than 7% for five measurements. The proposed method was successfully implemented for the determination of citalopram in human plasma and urine samples.     

Multi-Pesticide Analysis in Sediment by GC-EI-MS/MS Using Programmed Temperature Vaporization–Large Volume Injection Technique

A sensitive, selective and high throughput gas chromatography–tandem mass spectrometry method using programmable temperature vaporization–large volume injection mode (PTV-LVI-GC-MS/MS) for the analysis of 30 organochlorine pesticides (OCPs) including toxaphenes in sediments was developed. The PTV-LV injection settings, viz. inlet temperature, split flow, injection phase time, and injection speed were optimized for 50 µL injection. A significant increase in sensitivity was accomplished as compared with that obtained by the conventional 1 µL cold splitless injection. Average LVI recoveries for OCPs were in the range 58–133 % with low % RSD in instrument precision (<12 %). The method detection limits achieved were 0.04–0.92 µg kg^?1. The method recovery ranged from 80 to 120 % with <10 % RSD for more than 83 % of targeted analytes fortified at 10 µg kg^?1 in sediments. The PTV-LVI-GC-MS/MS allows simultaneous determination and unambiguous confirmation of trace OCPs and toxaphene congeners, which significantly streamlines and improves the trace organic analysis in the environmental surveillance and monitoring.     

Multiwalled Carbon Nanotube Coated on Stainless Steel Wire for Solid-Phase Microextraction of Organochlorine Pesticides in Water

A novel solid-phase microextraction (SPME) fiber was prepared by coating multiwalled carbon nanotube (MWCNTs) on a stainless steel wire, and its characteristics were studied. To evaluate the MWCNTs coating, the fiber was used for the extraction of some organochlorine pesticides (OCPs) from water samples by Headspace SPME (HS-SPME) mode. Potential factors affecting the extraction efficiency such as extraction time, extraction temperature, agitation, ionic strength, desorption temperature, and time were also optimized. Several experiments were carried out by water spiked with target compounds to evaluate the analytical characteristics of the proposed method under optimized conditions. The linearity was from 0.1 to 10 ug/L with the linear correlation coefficients (r) ranging from 0.9956 to 0.9995. The limits of detection (LOD, S/N = 3) for these pesticides were between 0.43 and 2.13 ng/L and the precision (RSD, n = 5) was 2.53–12.25%. When this method was applied for the spiked real river sample, the relative recoveries ranged from 72.4% to 134.7% for the tested OCPs.     

Experimental Design Optimization of Solid‐Phase Microextraction Conditions for the Determination of Heterocyclic Aromatic Amines by High‐Performance Liquid Chromatography

Abstract

Solid‐phase microextraction, using Carbowax‐Templated Resin fiber, coupled with high performance liquid chromatography ultra violet/diode array detector (HPLC‐UV/DAD) has been optimized for the determination of the heterocyclic aromatic amines (HAs). Three variables (absorption time, soaking time, and desorption time) were considered as factors in the optimization process. Interactions between analytical factors and their optimal levels were investigated using two level factorial and Doehlert matrix designs. Absorption time and soaking time were significant variables, and 15 min for each one of the variables was chosen for the best response. The optimized procedure allowed the determination of HAs with detection limits that ranged from 1.58 to 16.8 ng/L (except PhIP: 23.8 ng/L). The reproducibility of the method (n=5), expressed as relative standard deviation was between 2.21% and 28.3%. The method was applied to the analysis of a meat extract sample and the range of recoveries for the amines was 64.14%–112.72%.     

Homogeneous Liquid–Liquid Microextraction for Determination of Organochlorine Pesticides in Water and Fruit Samples

A fast and effective preconcentration method for extraction of organochlorine pesticides (OCPs) was developed using a homogeneous liquid–liquid extraction based on phase separation phenomenon in a ternary solvent (water/methanol/chloroform) system. The phase separation phenomenon occurred by salt addition. After centrifugation, the extraction solvent was sedimented in the bottom of the conical test tube. The OCPs were transferred into the sedimented phase during the phase separation step. The extracted OCPs were determined using gas chromatography–electron capture detector. Several factors influencing the extraction efficiency were investigated and optimized. Optimal results were obtained at the following conditions: volume of the consolute solvent (methanol), 1.0 mL; volume of the extraction solvent (chloroform), 55 μL; volume of the sample, 5 mL; and concentration of NaCl, 5 % (w/v). Under optimal conditions, the preconcentration factors in the range of 486–1,090, the dynamic linear range of 0.01–100 μg L^?1, and the limits of detection of 0.001–0.03 μg L^?1 were obtained for the OCPs. Using internal standard, the relative standard deviations for 1 μg L^?1 of the OCPs in the water samples were obtained in the range of 4.9–8.6 % (n = 5). Finally, the proposed method was successfully applied for extraction and determination of the OCPs in water and fruit samples.     

Gas chromatography–triple quadrupole tandem mass spectrometry: a powerful tool for the (ultra)trace analysis of multiclass environmental contaminants in fish and fish feed

A new method for rapid determination of 73 target organic environmental contaminants including 18 polychlorinated biphenyls, 16 organochlorinated pesticides, 14 brominated flame retardants and 25 polycyclic aromatic hydrocarbons in fish and fish feed using gas chromatography coupled with triple quadrupole tandem mass spectrometry (GC–MS/MS) was developed and validated. GC–MS/MS in electron ionization mode was shown to be a powerful tool for the (ultra)trace analysis of multiclass environmental contaminants in complex matrices, providing measurements with high selectivity and sensitivity. Another positive aspect characterizing the newly developed method is a substantial simplification of the sample preparation, which was achieved by an ethyl acetate QuEChERS (quick, easy, cheap, effective, rugged and safe) based extraction followed by silica minicolumn clean-up. With use of this sample preparation approach the sample laboratory throughput was increased not only because six samples may be prepared in approximately 1 h, but also because all the above-mentioned groups of contaminants can be determined in a single GC–MS/MS run. Under the optimized conditions, the recoveries of all target analytes in both matrices were within the range from 70 to 120 % and the repeatabilities were 20 % or less. The method quantification limits were in the range from 0.005 to 1 μg kg^–1 and from 0.05 to 10 μg kg^–1 for fish muscle tissue and fish feed, respectively. The developed method was successfully applied to the determination of halogenated persistent organic pollutants and polycyclic aromatic hydrocarbons in fish and fish feed samples.     

Simultaneous determination of three organophosphorus pesticides in different food commodities by gas chromatography with mass spectrometry

A sensitive and selective gas chromatography with mass spectrometry method was developed for the simultaneous determination of three organophosphorus pesticides, namely, chlorpyrifos, malathion, and diazinon in three different food commodities (milk, apples, and drinking water) employing solid‐phase extraction for sample pretreatment. Pesticide extraction from different sample matrices was carried out on Chromabond C₁₈ cartridges using 3.0 mL of methanol and 3.0 mL of a mixture of dichloromethane/acetonitrile (1:1 v/v) as the eluting solvent. Analysis was carried out by gas chromatography coupled with mass spectrometry using selected‐ion monitoring mode. Good linear relationships were obtained in the range of 0.1–50 μg/L for chlorpyrifos, and 0.05–50 μg/L for both malathion and diazinon pesticides. Good repeatability and recoveries were obtained in the range of 78.54–86.73% for three pesticides under the optimized experimental conditions. The limit of detection ranged from 0.02 to 0.03 μg/L, and the limit of quantification ranged from 0.05 to 0.1 μg/L for all three pesticides. Finally, the developed method was successfully applied for the determination of three targeted pesticides in milk, apples, and drinking water samples each in triplicate. No pesticide was found in apple and milk samples, but chlorpyrifos was found in one drinking water sample below the quantification level.     

Polymer Monolith Microextraction Coupled with HPLC for Determination of Jasmonates in Wintersweet Flowers

A simple, fast, and effective method has been presented for the determination of jasmonates in plant samples by polymer monolith microextraction (PMME). A poly (methacrylic acid-ethylene glycol dimethacrylate) (MAA-EGDMA) monolith-based device was developed for extraction, purification, and concentration; HPLC-UV was used for evaluation. To realize the best microextraction efficiency, parameters such as sample pH value, flow rate, and sample volume were systematically examined and optimized. Aqueous solution (5 mL) of jasmonates at pH 3.0 was selected as sample solution, and loaded onto the monolith at flow rate of 0.15 mL/min; finally, 50 μL of acetonitrile was used for elution. The proposed method exhibited impressive enrichment efficiency (almost 100-fold) and the limits of detection for jasmonic acid and methyl jasmonate obtained 0.5 and 2 ng/mL by using UV detection. Wide linear ranges were also observed (2–2000 and 5–2000 ng/mL) for both jasmonic acid and methyl jasmonate, with R² > 0.999. The developed PMME-HPLC method was successfully applied to the determination of jasmonates in fresh wintersweet flowers with recoveries in the range of 91.9–97.2%. The result was confirmed by an HPLC-MS method. The PMME method was also compared with a conventional C18-SPE method and exhibited better clean-up efficiency.     

A new sensitive method for the quantification of glyoxal and methylglyoxal in snow and ice by stir bar sorptive extraction and liquid desorption-HPLC-ESI-MS

In this study, the development of a new sensitive method for the analysis of alpha-dicarbonyls glyoxal (G) and methylglyoxal (MG) in environmental ice and snow is presented. Stir bar sorptive extraction with in situ derivatization and liquid desorption (SBSE-LD) was used for sample extraction, enrichment, and derivatization. Measurements were carried out using high-performance liquid chromatography coupled to electrospray ionization tandem mass spectrometry (HPLC-ESI-MS/MS). As part of the method development, SBSE-LD parameters such as extraction time, derivatization reagent, desorption time and solvent, and the effect of NaCl addition on the SBSE efficiency as well as measurement parameters of HPLC-ESI-MS/MS were evaluated. Calibration was performed in the range of 1–60 ng/mL using spiked ultrapure water samples, thus incorporating the complete SBSE and derivatization process. 4-Fluorobenzaldehyde was applied as internal standard. Inter-batch precision was <12 % RSD. Recoveries were determined by means of spiked snow samples and were 78.9?±?5.6 % for G and 82.7?±?7.5 % for MG, respectively. Instrumental detection limits of 0.242 and 0.213 ng/mL for G and MG were achieved using the multiple reaction monitoring mode. Relative detection limits referred to a sample volume of 15 mL were 0.016 ng/mL for G and 0.014 ng/mL for MG. The optimized method was applied for the analysis of snow samples from Mount Hohenpeissenberg (close to the Meteorological Observatory Hohenpeissenberg, Germany) and samples from an ice core from Upper Grenzgletscher (Monte Rosa massif, Switzerland). Resulting concentrations were 0.085–16.3 ng/mL for G and 0.126–3.6 ng/mL for MG. Concentrations of G and MG in snow were 1–2 orders of magnitude higher than in ice core samples. The described method represents a simple, green, and sensitive analytical approach to measure G and MG in aqueous environmental samples.     

Online solid-phase extraction–liquid chromatography–electrospray–tandem mass spectrometry determination of multiple classes of antibiotics in environmental and treated waters

An online solid-phase extraction and liquid chromatography in combination with tandem mass spectrometry method was developed for the simultaneous determination of 31 antibiotics in drinking water, surface water and reclaimed waters. The developed methodology requires small sample volume (10 mL), very little sample preparation and total sample run time was 20 min. An Ion Max API heated electrospray ionization source operated in the positive mode with two selected reaction monitoring transitions was used per antibiotic for positive identity and quantification performed by the internal standard approach, to correct for matrix effects and any losses in the online extraction step. Method detection limits were in the range of 1.2–9.7, 2.2–15, 5.5–63 ng/L in drinking water, surface water and reclaimed waters, respectively. The method accuracy in matrix spiked samples ranged from 50–150 % for the studied antibiotics. The applicability of the method was demonstrated using various environmental and reclaimed water matrices. Erythromycin was detected in more than 85 % of the samples in all matrices (28–414, n.d.–199, n.d.–66 ng/L in reclaimed, river and drinking waters respectively). The other frequently detected antibiotics in reclaimed waters were nalidixic acid, clarithromycin, azithromycin, trimethoprim, and sulfamethoxazole.     

Fully automated standard addition method for the quantification of 29 polar pesticide metabolites in different water bodies using LC-MS/MS

A reliable quantification by LC-ESI-MS/MS as the most suitable analytical method for polar substances in the aquatic environment is usually hampered by matrix effects from co-eluting compounds, which are unavoidably present in environmental samples. The standard addition method (SAM) is the most appropriate method to compensate matrix effects. However, when performed manually, this method is too labour- and time-intensive for routine analysis. In the present work, a fully automated SAM using a multi-purpose sample manager “Open Architecture UPLC®-MS/MS” (ultra-performance liquid chromatography tandem mass spectrometry) was developed for the sensitive and reliable determination of 29 polar pesticide metabolites in environmental samples. A four-point SAM was conducted parallel to direct-injection UPLC-ESI-MS/MS determination that was followed by a work flow to calculate the analyte concentrations including monitoring of required quality criteria. Several parameters regarding the SAM, chromatography and mass spectrometry conditions were optimised in order to obtain a fast as well as reliable analytical method. The matrix effects were examined by comparison of the SAM with an external calibration method. The accuracy of the SAM was investigated by recovery tests in samples of different catchment areas. The method detection limit was estimated to be between 1 and 10 ng/L for all metabolites by direct injection of a 10-μL sample. The relative standard deviation values were between 2 and 10 % at the end of calibration range (30 ng/L). About 200 samples from different water bodies were examined with this method in the Rhine and Ruhr region of North Rhine-Westphalia (Germany). Approximately 94 % of the analysed samples contained measurable amounts of metabolites. For most metabolites, low concentrations ≤0.10 μg/L were determined. Only for three metabolites were the concentrations in ground water significantly higher (up to 20 μg/L). In none of the examined drinking water samples were the health-related indication values (between 1 and 3 μg/L) for non-relevant metabolites exceeded.