Quick Polar Pesticides Research Articles

BİTKİSEL KÖKENLİ GIDALARDA YÜKSEK POLARİTELİ PESTİSİTLERİN SIVI KROMATOGRAFİ/KÜTLE SPEKTROMETRİSİ YÖNTEMİYLE ANALİZİ

Pesticides in foods of plant origin are becoming a major issue due to their intensive use in agriculture. Since pesticides are potentially harmful to the environment and consequently to human health through the consumption of pesticide contaminated foods. The European Community and also the Ministry of Agriculture and Forestry in Turkish Republic established maximum residue levels (MRLs), based on the assumption that good agricultural practice is applied at the use of pesticides in farming, for pesticide residues in food of plant origin. As a consequence food commodities have to be controlled to assure the non-violation of the MRLs. Thus an appropriate control of their residues in samples has to be operated. 
 In this study, we inferred the analytical methods for highly polar pesticides in foods of plant origin via LC-MS/MS after extraction with acidified methanol according to QuPPe (Quick Polar Pesticides) method. Optimization of 13 highly polar pesticides was carried out with LC-MS/MS Q-Trap. After the optimization process has been completed, the samples to be taken according to the SANTE (Guidance document on analytical quality control and method validation procedures for pesticide residues and analysis in food and feed) guidelines have been carefully selected, including high water, high acid/high water, high sugar/low water, high oil/low water and high starch/low water content and difficult or unique commodities. Six samples carefully selected according to the SANTE guideline were carried out at two different concentrations, one of at the detection limit which is 10 µg/L. At the end of the studies, it was found that the RSD criteria for repeatabilitiy was below 20 % for all substances. In addition, the recovery value for all substances was in the range of 70 – 120 %. As a result, 13 different polar pesticides can be analyzed in product groups of plant origin via LC-MS/MS method developed by using hypercarb column.

Pesticide Residues in Mandarins: Three-Year Monitoring Results.

The demand of plant production product use has increased because of the current system of citrus production, which prioritizes high agricultural yields. Therefore, the monitoring of pesticide residues in citrus fruits and other agricultural products and their impacts on human health and food security are of great concern. This study aims to determine multi-class pesticides including highly polar residues in satsuma mandarins. A total of 226 mandarin samples were collected over three consecutive harvesting years from 2019 to 2021 in the Izmir region of Turkey. Targeted compounds included pesticides and metabolites with European Union (EU) regulatory levels, plus other non-approved residues and highly polar compounds. The residues excluding highly polar substances were analyzed by applying the quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction and liquid chromatography-triple quadrupole mass spectrometry (LC-MS/MS) determination for 434 analytes and gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS) determination for 71 analytes. For six highly polar pesticides, sample preparation was based on Quick Polar Pesticides (QuPPe) extraction. The polar residues were determined by LC-MS/MS using internal standards. Forty different residues, including two highly polar substances, were recorded in mandarin samples through three harvesting years. In 8.4% of the samples, no quantifiable residues were detected, whereas 207 samples contained at least one residue. The maximum residue level (MRL) exceedances were recorded for 22.1% of the samples. The two most frequently found pesticides were phosphonic acid and spirotetramat, with an incidence rate of 48.7% and 46.5%, respectively. The concentration of phosphonic acid and spirotetramat in mandarin samples varied from 0.026 to 39.386 mg kg-1 and from 0.010 to 1.485 mg kg-1, respectively. The results will enable researchers and regulatory authorities to assess the extent of pesticide presence, identify potential risks, and take necessary measures to ensure the safety of satsuma mandarins for consumers.

Monitoring and Exposure Assessment of Fosetyl Aluminium and Other Highly Polar Pesticide Residues in Sweet Cherry.

Cherries are popular fruits due to their health benefits, organoleptic quality, and attractive appearance. Since highly polar pesticides are of low mass and amphoteric character, and are not amenable to traditional multi-residue extraction methods, they are more commonly not included in the pesticide monitoring program. This study aims to determine twelve highly polar pesticide residues in cherry samples intended for export from Turkey. A total of 16,022 cherry samples from 2018-2020 harvests in four production areas of Turkey were analyzed using a modification of the Quick Polar Pesticides method and liquid chromatography-tandem mass spectrometry. The method was validated at two fortification levels (0.01 and 0.05 mg kg-1), and good recoveries (87.4-111.4%) and relative standard deviations (<6%) were achieved for all analytes. The limits of quantification were in the range of 1.08-2.55 μg kg-1. Overall, 28.4% of the analyzed cherry samples were detected with phosphonic acid, calculated as fosetyl aluminium (fosetyl-Al) in amounts up to 77.7 mg kg-1. For 2304 samples (14.4%), the residues exceeded the European Union maximum residue level of 2 mg kg-1. There is no reason to be concerned about long-term exposure to phosphonic acid/fosetyl-Al, and the other highly polar pesticides through the consumption of sweet cherry.

Analysis of highly polar pesticides in foods by LC-MS/MS.

Highly polar pesticides (HPP) are a group of pesticides that are characterize as low Log Kow. Many high-throughput multi-residue analysis methods based on liquid chromatography-tandem mass spectrometry (LC-MS/MS) for the simultaneous determination of such polar pesticides have been proposed. In this article, we summarize the various sample preparation methods including quick polar pesticides (QuPPe), dispersive solid phase extraction (dSPE), solid phase extraction (SPE) and QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe), especially for QuPPe, which are mainly used for the determination of HPP in foods. In addition, we summarize LC-based separation methodologies that are currently used for the analysis of HPP in foods, including reversed-phase chromatography (RPC), hydrophilic interaction liquid chromatography (HILIC), ion chromatography (IC) and mixed-mode chromatography (MMC). Finally, the current mass spectrometry-based methodologies for the analysis of HPP are summarized with a specific focus on MS configurations and acquisition modes.

Direct determination of glyphosate, aminomethylphosphonic acid and glufosinate in food samples with ion chromatography coupled to electrospray ionization tandem mass spectrometry

A fast and reliable method for the direct determination of the herbicide glyphosate, its major degradation product aminomethylphosphonic acid (AMPA) and glufosinate is presented for a variety of food matrices. The Quick Polar Pesticides in food of Plant Origin method (QuPPe-PO-Method) was used for extraction without further preconcentration or clean-up steps involving e.g. solid phase extraction (SPE). The method makes use of a commercially available high performance liquid chromatograph coupled to a tandem mass spectrometer with electrospray ionization (LC-ESI-MS/MS) - as present in many laboratories - equipped with an ion chromatography (IC)-column using an MS-compatible eluent made of 0.8% formic acid in water. Due to the absence of time-consuming clean-up procedures, strong matrix effects (ME) of up to 91% for AMPA in grapefruit can be observed, when comparing its sensitivity to that obtained for solvent-based standards. The limits of detection (LODs) were determined for the sample matrices apple, mushrooms, grapefruit, linseed, red lentils and wheat and they were found to be in the range of 0.09 to 0.8, 0.04 to 1 and 0.2 to 2 µg/kg for glyphosate, AMPA and glufosinate, respectively. For the same matrices the validation was carried out according to SANTE guidelines for different commodity groups by spiking them up prior to extraction to concentrations ranging from 10 to 400 µg/kg for matrices with high water content and from 10 to 800 µg/kg for matrices with low water content. When using solvent-based calibration under the use of isotopically labelled internal standards (ILIS) the recoveries were found to range from 84% to 120% and the relative standard deviations (RSD) range between 1% and 19% for glyphosate, AMPA and glufosinate at all fortification levels for all matrices investigated. Accordingly, the method was successfully introduced in our laboratory with limits of quantification (LOQs) of 10 µg/kg for glyphosate, AMPA and glufosinate in samples from SANTE commodity groups 1, 2, 4a and 5. The reliability and robustness of the method are demonstrated by showing a recovery control chart obtained for glyphosate in randomly selected samples from different commodity groups. Therefore, the samples were spiked up with 10 µg/kg of glyphosate during routine analysis, whereby all recoveries were found to be in the range between 70 and 120%.

Development of a Quantitative Method for Detection of Multiclass Veterinary Drugs in Feed Using Modified QuPPe Extraction and LC-MS/MS.

A method was developed for the rapid and quantitative analysis of 30 veterinary drugs belonging to 17 classes (amphenicols (1), anthelmintics (1), cephalosporins (4), coccidiostats (1), lincosamides (1), macrolide (1), nitroimidazole (1), penicillins (3), phenylhydrazines (1), polypeptides (1), pyrethrins (1), quinolones (5), sulfonamides (3), tetracycline (3), neuroleptic agents (1), triazene trypanocidal agents (1), other. (1)) in feeds. The proposed method with a modified Quick Polar Pesticides (QuPPe) sample preparation was validated for the determination of 30 veterinary drugs in feed samples by liquid chromatography triple-quadrupole mass spectrometry (LC–MS/MS). The sample was extracted with methanol containing 1% acetic acid and purified by dispersive solid-phase extraction (d-SPE) with C18. Good linearity (r2 ≥ 0.98) was observed, and the LOQ values ranged from 10 to 200 µg/kg. Average recoveries ranged from 70.8 to 118.4%, and the relative standard deviation was ≤ 18.7%. This validated method was used in the determination of 30 veterinary drugs in 142 feed samples obtained from South Korea. The results show that lincomycin was present in only one of the tested feed samples, although it was detected at a value lower than the LOQ. In conclusion, this multi-residue method can be used for screening through the detection and quantitation of residual multiclass veterinary drugs in feed samples.

Quick Polar Pesticides (QuPPe): Learning from and Expanding on the Work of Others

In January, Steve Lehotay from the U.S. Department of Agriculture provided an update on the quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction method, originally developed for multiresidue pesticide analysis. Like any method, QuEChERS had some deficiencies, which were addressed with the new QuEChERSER (adding “efficient” and “robust” to the acronym) mega-method. Meanwhile, the European Union (EU) Reference Laboratories developed a new method for the multiresidue analysis of highly polar pesticides, called the quick polar pesticides (QuPPe) method. This month, we take a look at QuPPe, comparing and contrasting it with QuEChERS and noting how we can learn from previously developed methods as we strive for improvements.

Chlorate and perchlorate residues in food products on the Danish market

ABSTRACT Upon the European commission’s request in 2013, Denmark initiated a survey of the levels of chlorate and perchlorate in agriculture products from the Danish market over a period of 4 years from 2014 to 2017. The results of the survey were used to guide decision making with a view to setting maximum levels for intra-Union trade in 2013 and reviewing and updating the levels from 2020. The results of the Danish survey and the employed analytical method are documented in this paper. In addition to the 89 domestic samples, 30 samples of foreign origin were analysed for chlorate and perchlorate, together with ten samples of baby food and seven samples of infant formula collected from the Danish market. Samples were extracted using the Quick Polar Pesticides extraction method (QuPPe) and analysed on a triple quadrupole LC-MS/MS system. The levels of both chlorate and perchlorate detected in samples originating from Denmark were lower than the current MRLs except for a single sample of lettuce. Moreover, the percentage of foreign samples that were positive for chlorate and perchlorate residues was higher than the percentage of domestic samples. The reason for the generally low levels and low frequency of chlorate and perchlorate in Danish products is most likely linked to the fact that the water supply in Denmark is 100% unchlorinated ground water. The present study shows that residues of perchlorate and chlorate are found in Danish food products at a relatively low frequency and that the levels found are below the EU’s MRLs implemented in 2020.

A modified quick, easy, cheap, effective, rugged, and safe method for determination of by-products originating from ozonation of chlorpyrifos and diazinon spiked in cherry tomato and perilla leaf.

In this study, sample pretreatment methods have been developed for the determination of chlorpyrifos, diazinon, and their by-products present in cherry tomato and perilla leaf using liquid chromatography-tandem mass spectrometry. To optimize a quick, easy, cheap, effective, rugged, and safe method, the recoveries at each step were evaluated. The steps improved the recoveries of chlorpyrifos, chlorpyrifos oxon, diazinon, diazoxon, and 2-isopropyl-6-methyl-4-pyrimidinol up to 80% or more by removing interferents, but diethyl phosphate was almost lost during the partition procedure, and the 3,5,6-trichloro-2-pyridinol recovery was below 65%. Therefore, the compounds were evaluated using different solvent compositions based on a quick polar pesticides method; note that 100% methanol showed acceptable extraction results. The optimized method provided method detection limits ranging from 0.03 to 1.22ng/g and good linearities (R2 >0.996). The recovery values were between 82.1 and 113.3%. The intra- and interday reproducibility was evaluated to be within 8.6 and 9.9%, respectively. The method was applied to determine the degradation efficiency of chlorpyrifos and diazinon and their by-products formed during plasma treatment.

Monitoring of Paraquat in soya products intended for animal feed

Even though paraquat is considered to be one of the most toxic herbicides, it is one of the most used ones. Paraquat-based preparations are heavily used across many important agricultural countries and for a lot of types of crops such as soya. As soya is used in large quantities in the feed production, paraquat residues in soya products are a potential threat to livestock. The aim of this study was to investigate whether soya products intended for animal feed contain residues of paraquat. Therefore, an optimized Quick Polar Pesticides (QuPPe) Method was developed. In total, 174 samples were analyzed via LC-MS/MS using zwitterionic hydrophilic interaction liquid chromatography (ZIC-HILIC). The results showed that paraquat was detected in 66 % of the samples above 0.008 mg/kg. Residues were mainly present in soya bean meals that were imported from Brazil or the USA and cultivated using genetically modified soya. Around 5 % of the samples were not compliant with the European regulation on maximum residue levels of pesticides in or on food and feed. The results of this study support the view that paraquat residues play a significant role in soya products intended for animal feed and, thus, need to be controlled on a regular basis. However, for enforcement actions reliable processing factors for paraquat in soya products or maximum residue levels for processed soya products are urgently required.

A potential threat to black figs intended for export from Turkey: Ethephon

The analysis of highly polar pesticide residues in fruits and vegetables has become a controversial issue in the last decade. This report shows the results of highly polar pesticide residues (ethephon, fosetyl aluminium (fosetyl-Al) and phosphonic acid) monitoring on black figs intended for export from Turkey. From 2017–2020, a total of 9237 black fig samples were analysed for ethephon, fosetyl-Al and phosphonic acid residues using the Quick Polar Pesticides (QuPPe) method. The method has shown to have sufficiently low limits of quantification with respect to EU Maximum Residue Levels (MRLs). The obtained recovery and precision parameters fulfil the requirements in SANTE/11813/2017 Guideline. The 16.8 % of black fig samples were detected with ethephon at quantifiable concentrations but below the EU MRL of 3 mg kg−1. The concentration of ethephon ranged between 0.005 and 2.47 mg kg−1. However, no quantifiable residues of fosetyl-Al and phosphonic acid were detected in any black fig samples.

LC-MS/MS characterisation and determination of dansyl chloride derivatised glyphosate, aminomethylphosphonic acid (AMPA), and glufosinate in foods of plant and animal origin

Glyphosate and other polar and acidic pesticides have been particularly studied due to the concerns over widespread and intensive use. The chemical properties of these compounds necessitate use of customised methods, such as derivatisation or ion exchange chromatography. These approaches present a compatibility problem with ESI-MS due to presence of salts and non-volatile compounds. For that reason, a simple procedure has been developed for the extraction, pre-column derivatisation with dansyl chloride (5-(dimethylamino)naphthalene-1-sulfonyl chloride), and mass spectrometric detection of glyphosate, AMPA, and glufosinate after the separation on a C18stationary phase. The dansyl derivatives were characterised with ESI-MS and their separation from derivatisation reagent byproducts was demonstrated with UV absorption detection. Reagent byproducts eluted before the analytes and were separated from the analytes completely, thus the proposed procedure did not contaminate the mass spectrometers. The proposed procedure was evaluated with respect to the matrix effects and extraction efficiency, and was validated with different mass spectrometers for milk, cucumber, honey, porridge formula, bovine kidney and liver matrix. The LOQ was 10 μg kg−1 for AMPA and glufosinate, and 10–25 μg kg−1for glyphosate, depending on matrix. Measurement uncertainties ranged from 4 to 44%. Method performance was compared to the QuPPe (Quick Polar Pesticides) procedure in combination with a diethylamino-based column from Waters™. In the case of Orbitrap™ detection, the proposed procedure had a comparable performance to the QuPPe procedure. Although, improved peak shape, higher absolute peak intensity, and lower standard deviation of the calibration curve slope was observed with the proposed procedure. This could be explained by the superior electrospray stability and lower extent of ion suppression.

Quantification of fosetyl-aluminium/phosphonic acid and other highly polar residues in pomegranates using Quick Polar Pesticides method involving liquid chromatography-tandem mass spectrometry measurement

Interest in the quantification of highly polar substances in crops has noticeably increased in the last five years. This study was designed to assess quantification of six polar residues, chlorate, ethephon, fosetly-aluminium (fosetyl-Al), glyphosate, phosphonic acid and perchlorate. A total of 2513 pomegranate samples intended for export from Turkey were analysed using the Quick Polar Pesticides (QuPPe) method. The method was in-house validated with very good performance results. The limits of quantification (LOQs) for residues were much lower than the respective EU Maximum Residue Levels (MRLs). Phosphonic acid was detected in 38.5% of pomegranate samples at quantifiable concentrations, calculated as fosetyl-Al. The concentrations ranged between 0.005 and 12.9 mg kg−1. The 20% of pomegranate samples showed fosetyl-Al levels above the EU MRL of 2 mg kg−1. Other polar residues were not detected in any pomegranate samples. This is the first report about highly polar pesticides in pomegranates cultivated in Turkey.

Validation of Quick Polar Pesticides (QuPPe) Method for Determination of Eight Polar Pesticides in Cherries by LC-MS/MS

A novel and sensitive chromatography method with modified Quick Polar Pesticide (QuPPe) sample preparation was validated for determination of eight high polar pesticides in cherries by liquid chromatography-triple quadrupole mass spectrometry (LC-MS/MS). The validation data executed the conditions of the European SANTE/12682/2019 Guidance Document. Good linearity (R2 > 0.99) was observed, and the residuals were lower than ± 20%. Average recoveries ranged from 70.2 to 105.1%, and LOQ values ranged from 1.77 to 12.13 μg kg−1. The repeatability and reproducibility are in range of 1.57–15.56% and 3.51–16.17% separately. All measurement uncertainty values were lower than 50% for all polar pesticides. This verified analytical method was used to detect pesticide residue levels of cherries, and none of the eight high polar pesticides were found in 225 real samples. This is the first validation report of QuPPe sample preparation and LC-MS/MS method of high polar pesticide residues in cherries from Turkey.

Monitoring of polar pesticides and contaminants in edible oils and nuts by liquid chromatography-tandem mass spectrometry

A single method was developed for the determination of polar pesticides (fosetyl-Al and its metabolite, phosphonic acid, and ethephon) and environmental contaminants (chlorate and perchlorate) in edible oils and nuts. Two extraction methods based on QuPPe-PO approach (Quick Polar Pesticides Method for products of Plant Origin) were optimized. In oils, a single extraction using water acidified with formic acid (1%) was performed, while in nuts, the clean-up step was modified. C18 was used as sorbent and an extra cleaning step with n-hexane was added. The extracts were analysed by liquid chromatography coupled to a triple quadrupole mass analyser (LC-QqQ-MS/MS). The method was validated and the limit of quantification was 0.01 mg kg−1 for all analyte-matrix combination. Recoveries from 70 to 120%, and intra and inter-day precision values ≤20% were obtained. Forty samples of edible oils and nuts were analysed, detecting phosphonic acid in nuts at concentrations up to 4.6 mg kg−1.

Rapid and reliable detection of glyphosate in pome fruits, berries, pulses and cereals by flow injection – Mass spectrometry

A flow injection – mass spectrometry method for rapid glyphosate detection in food commodities was developed and validated. The sample preparation protocol included a simple and rapid extract purification step through polymeric solid phase extraction cartridges followed by addition of isotopically labeled glyphosate to the final test sample. The optimized method was subjected to intra-laboratory validation (spiking range 0.5–100 mg/kg) in chickpeas, grapes and apples, as representatives of three different commodity groups as defined in SANTE/11813/2017 guidelines. Recoveries were in the range 60–111%, repeatability and within laboratory reproducibility were ≤17%.The trueness of the results generated with the developed method was evaluated by analysis of a set of incurred chickpea and wheat samples (glyphosate range 0.5–36 mg/kg) and comparison with the reference method (Quick Polar Pesticides Method), confirming the method fitness-for-purpose of rapid compliance testing.

Ethephon and fosetyl residues in fruits from São Francisco Valley, Brazil

ABSTRACTThis survey describes the occurrence of Ethephon (ETH) and Fosetyl in fruits intended for export produced in the São Francisco Valley, Brazil. The determination of these compounds was carried out by the QuPPe-method (Quick Polar Pesticides Method), which was optimised and successfully validated according to the SANTE/11813/2017. From January 2016 to December 2018 a total of 1048 samples were analysed for ETH residues. In 547 (53%) of the samples, residues below the EU MRL of 1 mg kg−1 were present. In 17 samples (2%) ETH residues were above 1 mg kg−1. Overall, the mean ETH level decreased after 2016. Analyses of fosetyl showed that (18%) of 109 mango samples were positive for this compound. Phosphonic acid was found in concentrations ranging from 0.12 to 3.2 mg kg−1 and 5% of the measurements were above the EU MRL of 2 mg kg−1. The results emphasise the quality control of fruits produced in this region.

Simultaneous determination of the quaternary ammonium pesticides paraquat, diquat, chlormequat, and mepiquat in barley and wheat using a modified quick polar pesticides method, diluted standard addition calibration and hydrophilic interaction liquid chromatography coupled to tandem mass spectrometry

In this study, a modified Quick Polar Pesticides (QuPPe) method, optimized by a central composite design, was developed to determine quaternary ammonium pesticides (QUATs) residues in barley and wheat by ultra-high-performance liquid chromatographic tandem mass spectrometry (UHPLC-MS/MS) using a hydrophilic interaction chromatography (HILIC) column. Considering the high polarity of these compounds, special conditions of sample preparation and analysis are required. Different mobile phases, extraction procedure and clean-up were evaluated. An isocratic elution with aqueous solution of ammonium formate 60 mmol L−1 (pH 3.7) and acetonitrile, 40:60 (v/v), was selected. Water and acidified methanol as extraction solvent, without heating, and a clean-up with dichloromethane, chitosan and acetonitrile presented good results. The validated method presented satisfactory selectivity, linearity, matrix effect, trueness and precision, providing recoveries from 93 to 110% with RSD < 13% for barley, and 70 to 115% with RSD < 18% for wheat. The complexity of these matrices requires the calibration in matrix and the diluted standard addition calibration (DSAC) procedure has been shown to be an excellent option to compensate for the matrix effect and the losses of the analytes in the extraction. Real samples of barley and wheat were analyzed and 60% presented concentrations of paraquat above the maximum limits allowed by the European Union. The modified QuPPe method combined with DSAC and HILIC-UHPLC-MS/MS demonstrated to be an effective approach to determine QUATs in barley and wheat, and is a good alternative for routine analysis. The use of the biosorbent chitosan is effective, low cost and more ecological when compared to others conventional sorbents.

Sensitive and rapid determination of glyphosate, glufosinate, bialaphos and metabolites by UPLC–MS/MS using a modified Quick Polar Pesticides Extraction method

Phosphoric acid-containing amino acid pesticides, including glyphosate, glufosinate, and bialaphos, have been frequently encountered in human poisoning and suicidal cases, thus a quick and sensitive determination method for these compounds is very important. Herein we report a sensitive and rapid method for the determination of glyphosate, glufosinate, bialaphos and their metabolites, aminomethylphosphonic acid (AMPA) and 3-methylphosphinicopropionic acid (MPPA) in human blood samples. The method involves extraction using a modified Quick Polar Pesticides Extraction (QuPPe) method, cleanup with the PRiME HLB sorbents and detection with ultra performance liquid chromatography coupled with tandem mass spectrometry (UPLC–MS/MS). The LODs were 0.02mg/L for glyphosate, glufosinate and AMPA, 0.01mg/L for bialaphos and MPPA, with the analysis time as short as ∼6min. To the best of our knowledge, the LODs are lower and the analysis time is shorter than previous reports on determination of these compounds in blood and serum samples. The method was successfully applied to the detection and quantification of glyphosate and AMPA for blood samples from real forensic cases. This extremely rapid determination method with high sensitivity is of significant importance, particularly for forensic cases where quick determination is vital.

Ion chromatography tandem mass spectrometry (IC-MS/MS) multimethod for the determination of highly polar pesticides in plant-derived commodities

A new sensitive, fast, and robust analytical method based on a QuPPe (Quick Polar Pesticides) extraction procedure coupled to ion chromatography-tandem mass spectrometry (IC-MS/MS) was developed. The study aimed at the determination of the highly polar pesticides chlorate, perchlorate, ethephon, and 2-hydroxyethylphosphonic acid (HEPA) in different plant food commodities. For achieving an acceptable dynamic range for chlorate and perchlorate and to compensate for matrix effects, the isotopically-labelled internal standards 18O3-chlorate and 18O4-perchlorate and ethephon D4 were applied for calibration. The optimized method was fully validated at levels of 0.010 and 0.100 mg kg−1 for all compounds in the matrices tomato, apple, lemon, sultana, avocado, and wheat according to the actual EU guidance document SANTE/11945/2015. For HEPA and the commodity sultana levels for validation were chosen at 0.050 mg kg−1 and 0.100 mg kg−1. The precision and accuracy of the validation results were determined at hand of five replicates with recovery rates between 93 and 119% and RSDs between 1 and 14%. The use of internal standards for chlorate, perchlorate and ethephon allows the determination in a wide working range between 0.01 and 1 mg kg−1 without interference by matrix effects. The developed analytical methodology is able to meet the strict requirements for the analysis of baby food.