Determination of seven pyrethroid pesticide residues in vegetables by gas chromatography using carboxylated multi-walled carbon nanotubes as dispersion solid phase extraction sorbent

ABSTRACT

A novel carboxylated multi-walled carbon nanotubes (MWCNTs-COOH) dispersive solid phase extraction (d-SPE) method combined with gas chromatography (GC) with an electron capture detector (ECD) was developed for the determination of seven pyrethroid pesticides in cucumber, spinach, eggplant, tomato and carrot. We optimised d-SPE conditions including the type and volume of the extractant, the type and amount of the sorbent, and shaking time. Under the optimal conditions, the linear range was from 2.0 to 2000 μg kg^?1. The recoveries were from 88.5% to 108.2%, with the corresponding RSDs <6%, correlation coefficients 0.9987–0.9998, LOD 0.5–2.9 μg kg^?1 and LOQ 1.5–9.7 μg kg^?1. The proposed method is simple, fast, and safe, with high recovery and sensitivity, and is applicable to analysis of pyrethroid pesticides in vegetable samples.     

Quantification of mycotoxins in vegetable oil by UPLC-MS/MS after magnetic solid-phase extraction

ABSTRACT

The detection of mycotoxin contamination in foodstuffs is highly significant for public health. Herein we report an analytical method based on magnetic solid-phase extraction (MSPE) and UPLC-MS/MS for the simultaneous determination of mycotoxins, including fumonisins B₁ (FB₁), zearalenone (ZON) and ochratoxin A (OTA), in vegetable oil. Magnetic nanoparticles coated with double layers of silicon dioxide were synthesised and found to be an effective MSPE adsorbent for mycotoxins. The proposed MSPE procedure serves not only for sample clean-up but also for mycotoxin enrichment that enhances greatly the assay’s sensitivity. Under the selected MSPE conditions, linear matrix-matched calibration curves were obtained for mycotoxins in a concentration range from 0.178 to 625 μg kg^–1. The limits of detection were 0.210 μg kg^–1 for FB₁, 0.0800 μg kg^–1 for OTA and 1.03 μg kg^–1 for ZON. The proposed MSPE UPLC-MS/MS method was applied for the determination of mycotoxins in vegetable oil samples, including maize oil, rapeseed oil and soybean oil. ZON was detected in a maize oil at 101 μg kg^–1, which is below the European Union limit of 200 μg kg^–1 in foodstuffs.     

Optimization of QuEChERS Procedure Coupled to GC-ECD for Organochlorine Pesticide Determination in Carrot Samples

An optimised version of the Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) method for simultaneous determination of 14 organochlorine pesticides in carrots was developed using gas chromatography coupled with electron-capture detector (GC-ECD) and confirmation by gas chromatography tandem mass spectrometry (GC-MS/MS). A citrate-buffered version of QuEChERS was applied for the extraction of the organochlorine pesticides, and for the extract clean-up, primary secondary amine, octadecyl-bonded silica (C18), magnesium sulphate (MgSO₄) and graphitized carbon black were used as sorbents. The GC-ECD determination of the target compounds was achieved in less than 20 min. The limits of detection were below the EU maximum residue limits (MRLs) for carrots, 10–50 μg kg^?1, while the limit of quantification did exceed 10 μg kg^?1 for hexachlorobenzene (HCB). The introduction of a sonication step was shown to improve the recoveries. The overall average recoveries in carrots, at the four tested levels (60, 80, 100 and 140 μg kg^?1), ranged from 66 to 111 % with relative standard deviations in the range of 2–15 % (n?=?3) for all analytes, with the exception of HCB. The method has been applied to the analysis of 21 carrot samples from different Portuguese regions, and β-HCH was the pesticide most frequently found, with concentrations oscillating between less than the limit of quantification to 14.6 μg kg^?1. Only one sample had a pesticide residue (β-HCH) above the MRL, 14.6 μg kg^?1. This methodology combines the advantages of both QuEChERS and GC-ECD, producing a very rapid, sensitive and reliable procedure which can be applied in routine analytical laboratories.     

Determination of Trichothecenes in Cereal Matrices Using Subcritical Water Extraction Followed by Solid-Phase Extraction and Liquid Chromatography-Tandem Mass Spectrometry

Subcritical water extraction followed by solid-phase extraction and ultra-high performance liquid chromatography coupled with tandem mass spectrometry detection is reported for the first time for the determination of 6 trichothecenes (deoxynivalenol, deoxynivalenol-3-glucoside, 3-acetyl-deoxynivalenol, 15-acetyl-deoxynivalenol, HT-2 toxin, and T-2 toxin) from different cereals. Water with 1% formic acid was used as the extraction solvent followed by a solid-phase extraction clean-up, achieving good performance with acceptable extraction recoveries, method detection limits between 0.05 μg kg^?1 and 4.0 μg kg^?1, and method quantification limits between 0.4 μg kg^?1 and 20 μg kg^?1. The use of water as the extraction solvent allowed a selective extraction affording low matrix effect levels and the detection and quantification of natural target trichothecenes at very low concentration levels. This extraction method was applied to different cereals, a pseudocereal and an oilseed sample, of which maize, millet, and oat were contaminated by at least one trichothecene.     

Gas Purge Microsyringe Extraction Coupled with Dispersive Liquid-Liquid Microextraction for the Determination of Acidic Compounds in Food Packaging Materials

A green, simple and sensitive method was developed for the analysis of volatile carboxylic acids (VFAs) and perfluorocarboxylic acids (PFCAs) in food packaging materials. The acidic compounds in food packaging materials were first extracted by gas purge microsyringe extraction (GP–MSE) with 1.0 mL 0.1 mol·L^?1 NaOH solution, then the analytes were dispersive liquid-liquid microextracted (DLLME) by 50 μL chloroform as extraction solvent and 200 μL acetonitrile as dispersive solvent. The 2-(5-Benzoacridine) ethyl-p-toluenesulfonate (BAETS) with excellent fluorescence property was applied to enhance the high performance liquid chromatography (HPLC) sensitivity. The obtained recoveries for the VFAs ranged from 92.0 to 101 %. The method LODs calculated at a signal-to-noise ratio (S/N) of 3 were in the range of 0.80–3.40 μg·kg^?1, while the LOQs calculated at S/N of 10 were in the range of 2.5–10.2 μg·kg^?1. All compounds were in good linearity with concentration coefficients of higher than 0.997. Perfluorooctanoic acid (PFOA) was found in all of the 15 kinds of samples analyzed with concentrations ranging from 4.86–7.56 μg·kg^?1. Acetic acid, butyric acid, and caprylic acid were found in half of the samples analyzed. The other analytes were also found in more than 30 % samples with concentrations varied between 3.96 and 293 μg·kg^?1.     

Ochratoxin A in red pepper flakes commercialised in Turkey

The aim of this study was to investigate the presence of Ochratoxin A (OTA) in red pepper flakes commercialised in Turkey. A total of 75 samples were collected from different supermarkets and traditional bazaars in Istanbul during 2012–2013. OTA analysis was performed by high-performance liquid chromatography equipped with fluorescence detection after immunoaffinity column clean-up. The method was linear in the range 0.05–40 μg kg^?1 (r² = 0.9997). Twenty-seven out of 31 (87.1%) packed red pepper flake samples contained OTA at concentrations ranging from 0.6 to 1.0 μg kg^?1, whereas 100% of the unpacked red pepper flake samples contained OTA, in the range 1.1–31.7 μg kg^?1. Overall, only 4 unpacked samples (5.3%) contained OTA, with a mean value of 23.4 μg kg^?1, which is higher than the European Union limit. It is suggested that OTA content should be carefully considered in red pepper flake samples especially marketed in unpacked form.     

Determination of Pesticide Residues in Golden Berry (<Emphasis Type="Italic">Physalis peruviana</Emphasis> L<Emphasis Type="Italic">.</Emphasis>) by Modified QuEChERS Method and Ultra-High Performance Liquid Chromatography-Tandem Quadrupole Mass Spectrometry

A fast and effective multiresidue method for the determination of 42 pesticides in golden berry was developed and validated. A modified QuEChERS method was established for sample preparation followed by ultra-high performance liquid chromatographic-tandem mass spectrometry (UHPLC-MS/MS) determination with electrospray ionization in a triple quadrupole system. Validation results were satisfactory, since the method presented recoveries between 70 and 114 % with relative standard deviations (RSD) <20 % for blank samples spiked from 5 to 25 μg kg^?1. The method limit of detection and limit of quantification were 1.5 and 5 μg kg^?1 _, respectively. Matrix effect ranged from ?32 to 218 % and was compensated using matrix-matched calibration. Method linearity was established from 2.5 to 100 μg kg^?1 with r ² ≥ 0.99. The proposed method combines the advantages of a simple and fast sample preparation step by a modified QuEChERS method with the high selectivity and sensitivity of the UHPLC-MS/MS system using selected reaction monitoring. The method was successfully applied to commercial samples, proving to be an efficient alternative for routine analysis. From the 16 analyzed samples, 13 presented residues of one or more pesticides (carbendazim, chlorpyrifos ethyl, dimethoate, propamocarb, and tebuconazole) in the concentration range of 2.0 to 55.6 μg kg^?1.     

Determination of Pydiflumetofen Residues in Some Foods of Plant and Animal Origin by QuEChERS Extraction Combined with Ultra-Performance Liquid Chromatography–Tandem Mass

A rapid and effective analytical method for determination of pydiflumetofen residues in some foods of plant and animal origin (grapes, tomatoes, wheat, pork, milk, and eggs) was developed using a modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) sample preparation procedure followed by ultra-performance liquid chromatography coupled with tandem mass spectrometry (UPLC–MS/MS). Acetonitrile was served as the extraction solvent, and an octadecylsilane-dispersive solid-phase extraction (C18-dSPE) was used to cleanup the analyte, and then detected by UPLC–MS/MS. Pydiflumetofen was eluted within 3.0 min from the HSS T3 chromatography column connected to an electrospray ionization source in positive mode. The linearity of the method was excellent (R²?≥?0.992) in the pydiflumetofen concentration range of 10–1000 μg kg^?1. The recoveries of spiked pydiflumetofen (10, 100, and 1000 μg kg^?1) from the matrices were satisfactory, being between 72.0 and 110.3%, and all with relative standard deviation values of <?15.1%. The limit of quantification for pydiflumetofen was 10 μg kg^?1. This study provides a method for the routine monitoring of pydiflumetofen.     

Determination of Triazoles in Tea Samples Using Dispersive Solid Phase Extraction Combined with Dispersive Liquid–Liquid Microextraction Followed by Liquid Chromatography–Tandem Mass Spectrometry

In this study, dispersive solid phase extraction (DSPE) combined with dispersive liquid–liquid microextraction (DLLME) method was developed for the determination of triazole fungicide residues in tea samples. DSPE with ODS C₁₈, primary secondary amine, and florisil as sorbents was applied to clean up and minimize matrix interference from tea samples; it was followed with the enrichment of target compounds in the DLLME procedure and detection with liquid chromatography–tandem mass spectrometry (LC-MS/MS). The effects of various experimental parameters on the DSPE and DLLME procedures were studied systematically, such as the kinds and volume of sorbents, extraction and dispersive solvents, and extraction time. Under optimum conditions, the method was validated in a tea matrix. The matrix-matched calibration curves of three triazoles had good linearity in the range of 0.0125–50 μg kg^?1, and the linear regression coefficients (r) ranged from 0.9998 to 0.9999. The limits of quantification (S/N?=?10) for penconazole, tebuconazole, and triadimenfon were 4.0, 7.8, and 31.6 ng kg^?1, respectively. The intra-day and inter-day relative standard deviations varied from 3.6 to 18.6 %. Recoveries in three concentration levels were between 91 and 118 %. The obtained results show that the proposed DSPE-DLLME-LC-MS method has the potential to analyze trace fungicides in a complex sample matrix.     

Optimization and Validation of a Method Without Alkaline Clean-Up for Patulin Analysis on Apple Puree Agar Medium (APAM) and Apple Products

A sensitive high-performance liquid chromatography-UV (HPLC-UV) method, based on the Association of Analytical Communities (AOAC) Official method 2000.02, was developed and validated for the high-throughput analysis of patulin in in vitro experiments on apple puree agar medium (APAM). The importance of repeating the ethyl acetate extraction step at liquid-liquid extraction (LLE) was examined, as well as the extent of patulin degradation during the sodium carbonate clean-up. In addition to this alkaline clean-up, the efficiency of using an Oasis HLB or C₁₈ cartridge as solid-phase extraction (SPE) clean-up was compared. This resulted in a two-step ethyl acetate LLE, followed by an Oasis HLB SPE clean-up, without alkaline clean-up conditions. The method was fully validated for APAM, cloudy apple juice, and apple puree. Average patulin recoveries at levels of 100, 500, and 1000 μg kg^?1 of APAM varied between 95 and 113 % over 3 independent days, with an interday precision (RSD_R) of 5 to 10 %. Recovery experiments carried out with the spiked apple juice (at 50 μg kg^?1) and apple puree (10 μg kg^?1) showed average recovery rates laying between 80–101 % (RSD_R?=?12 %) and 77–100 % (RSD_R?=?9 %), respectively. This method offered a detection limit of 3–4 μg kg^?1 and a quantification limit of 5–8 μg kg^?1 for APAM, apple juice, and puree.     

Simultaneous Determination of Eight Tranquilizers in Pork by Ultra-Performance Liquid Chromatography Coupled with Electrospray Tandem Mass Spectrometry

An ultra-performance liquid chromatography/electrospray ionization tandem mass spectrometry (UPLC-ESI-MS/MS) method was developed and validated for quantification of eight tranquillizers (chlorpromazine, imipramine hydrochloride, diazepam, nitrazepam, nordazepam, oxazepam, flurazepam, and haloperidol) in pork. Sample pretreatment consisted of extraction by acetonitrile, defatted by n-hexane, and further solid phase extraction by hydrophilic-lipophilic balance (HLB) extraction cartridges. The triple quadrupole mass spectrometer was operated in positive ion mode, and multiple reaction monitoring was used for drug quantification. The method was validated over the concentration ranges of 1.0 ～ 250 μg kg^?1 for the eight tranquillizers. The calibrations were performed in sample matrices, and the interference effect of sample matrices on the ionization was effectively eliminated. Good linear relationship (R ² > 0.99) was observed within the concentration range of 1.0–250 μg kg^?1. The average recoveries of the eight tranquillizers spiked at three levels ranged from 63.7 to103.2 % with the relative standard deviation below 11.8 %. The limits of detection were between 0.06 and 0.30 μg kg^?1, and the limits of quantification were between 0.2 and1.0 μg kg^?1 for all analytes in pork. This validated method has been successfully used to quantify the concentration of the eight tranquillizers in pork samples.     

Determination of glyphosate,AMPA, and glufosinate in honey by online solid-phase extraction-liquid chromatography-tandem mass spectrometry

A simple method was developed for the simultaneous determination of glyphosate, its main degradation product (aminomethylphosphonic acid), and glufosinate in honey. Aqueous honey solutions were derivatised offline prior to direct analysis of the target analytes using online solid-phase extraction coupled to liquid chromatography-tandem mass spectrometry. Using the developed procedure, accuracies ranging from 95.2% to 105.3% were observed for all analytes at fortification levels of 5, 50, and 150 μg kg^?1 with intra-day precisions ranging from 1.6% to 7.2%. The limit of quantitation (LOQ) was 1 μg kg^?1 for each analyte. Two hundred honey samples were analysed for the three analytes with AMPA and glyphosate being most frequently detected (99.0% and 98.5% of samples tested, respectively). The concentrations of glyphosate were found to range from <1 to 49.8 μg kg^?1 while those of its degradation product ranged from <1 to 50.1 μg kg^?1. The ratio of glyphosate to AMPA was found to vary significantly amongst the samples where both analytes were present above the LOQ. Glufosinate was detected in 125 of 200 samples up to a maximum concentration of 33.0 μg kg^?1.     

Determination of Polycyclic Aromatic Hydrocarbons (PAHs) in Olive and Refined Pomace Olive Oils with Modified Low Temperature and Ultrasound-Assisted Liquid–Liquid Extraction Method Followed by the HPLC/FLD

The cleanup method of modified low temperature was compared with the standardized method of modified ultrasound-assisted liquid–liquid (UALL) extraction for the analysis of 15 polycyclic aromatic hydrocarbons (PAHs) in olive oil and refined pomace olive oil. The modified UALL extraction consisted in purification on C₁₈ reversed-phase, Florisil-bonded-phase and NH₂ cartridges, and modified low-temperature extraction was followed by alumina-N and NH₂ solid-phase extraction (SPE) cartridges. Both methods are followed by reversed-phase high-performance liquid chromatography with fluorescence detection. The chromatograms of the final extracts showed lower interferences in both of the methods. The solvent consumption and cost for the modified UALL method were higher than those of the modified low temperature, and also, it needed more equipment, but its analysis time was less. The limit of detection and limit of quantitation of the modified UALL method were 0.16–0.97 and 0.57–2.93 μg kg^?1, respectively, and for the modified low temperature, they were 0.09–1.97 and 0.29–5.99 μg kg^?1, respectively. The PAH recoveries for the modified UALL extraction method ranged from 75.0 to 111.0 % (RSD?=?3–8 %), and for the modified low temperature, they ranged from 81.5 to 113.8 % (RSD?=?3–10 %).     

Co-occurrence of aflatoxins,ochratoxin A and citrinin in “egusi” melon (Colocynthis citrullus L.) seeds consumed in Ireland and the United Kingdom

The natural co-occurrence of aflatoxins (AFs), ochratoxin A (OTA) and citrinin (CIT) in melon seed samples obtained from retailers and households in Ireland and the United Kingdom (UK) was evaluated. AFs and OTA were determined by HPLC with fluorescence detection while CIT was analysed by HPLC-MS/MS. AFB₁ was detected in all (100%) samples (mean = 9.7 μg kg^?1; range = 0.2–66.5 μg kg^?1). Mean total AFs was 12.0 μg kg^?1 (range = 0.3–82 μg kg^?1). Commercially retailed samples showed a significantly higher AFB₁ contamination (p < 0.05) than the household samples. OTA occurred in 3 (13.6%) samples, while 4 (18.2%) were contaminated with CIT at very low levels. In this study, 68% of the melon seed samples were contaminated above the 2 μg kg^?1 EU limit for AFB₁ in oilseeds. These results highlight the need for the development of strategies to reduce AF contamination in “egusi” for human consumption.     

Deposition and depletion of maduramicin residues in eggs after oral administration to laying hens determined by LC-MS

The coccidiostat maduramicin has been approved as a feed additive for chickens and turkeys, although it is prohibited for use in laying hens. In the present study, laying hens were divided into three groups and fed for 14 days with medicated feed containing maduramicin, at three different concentrations: 50, 100 and 500 µg kg^?1. Eggs were collected during treatment and for 26 days after the end of feeding with medicated feed. Maduramicin residues were found exclusively in egg yolk, with the highest concentration in egg yolk of 459 µg kg^?1 for the highest dose. The maximum concentration of maduramicin in whole egg was 16.6 µg kg^?1 for the group receiving feed containing the maximum permitted level of maduramicin in feed (50 µg kg^?1). The half-life of elimination of maduramicin, calculated for post-treatment days 1–10, was 6.5 days. Twelve days after drug administration, the concentration of the maduramicin in egg yolk for Group 3 (fed with 500 µg kg^?1 maduramicin) still exceeded 20 µg kg^?1, while the concentrations for Groups 1 and 2 were 1.2 and 2.7 µg kg^?1, respectively.     

Concentrations and health hazards of polycyclic aromatic hydrocarbons in selected commercial brands of milk

The concentrations and profiles of polycyclic aromatic hydrocarbons (PAHs) were determined in twenty popular commercial brands of milk in the Nigerian market after saponification with ethanolic KOH and cyclohexane extraction and clean up using a gas chromatography with flame ionization detection. The concentrations of the Σ16 PAHs in these brands of milk ranged from 15.6 to 1,711.8 μg kg^?1. The dominant PAH compounds in these brands of milk were 3-and-4-rings PAHs. The dietary intake of BaP, PAH2, PAH4 and PAH8 were 0–53.9 and 0–369.6 ng kg^?1 bw day^?1 respectively. Using these indicators for occurrence and effects (BaP, PAH2, PAH4 and PAH8) PAHs in food, the margin of exposure were <10,000 in 15–30 % of the brands.     

Simultaneous Determination of Multiclass Pesticides and Antibiotics in Honey Samples Based on Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry

A simple, fast, and efficient method was developed for simultaneous determination of 79 pesticides and 13 antibiotics compounds of different chemical classes of pesticides and antibiotics in honey samples by ultra-high performance liquid chromatography with tandem mass spectrometry (UHPLC-MS/MS). The sample preparation procedure includes homogenization with McIlvaine buffer 0.1 mol L^?1 (pH 4), followed by extraction with acetonitrile and cleanup with florisil, using dispersive solid phase extraction (d-SPE). The proposed method was validated with good results, such as linearity (r ²?>?0.9901), normality, and independence of the evaluated data, as well as recoveries between 70 and 120 % with relative standard deviation (RSD) <20 % for most of the compounds spiked from 0.1 to 200 μg kg^?1. The experimental method limits of detection and quantification were from 0.03 to 1.51 μg kg^?1 and from 0.1 to 5 μg kg^?1, respectively, for the pesticides. For the antibiotics, the decision limits (0.1 to 2 μg g^?1) and the detection capacity (0.12 to 2.81 μg g^?1) were below the maximum residue limits (MRLs) established for honey by the Brazilian and European legislation. The method was successfully applied to real samples from different botanical and geographic origins. From them, 44 % presented residues from 0.12 to 10 μg kg^?1 of one or more analytes. The proposed method combines the advantages of a quick sample preparation step with the selectivity and sensitivity of the UHPLC-MS/MS and proved to be suitable for routine analyses.     

Aflatoxins and ochratoxin A in export quality raisins collected from different areas of Pakistan

During 2012–2014, 170 samples of export quality raisins were collected from different vendors in Pakistan. The collected samples were analysed for the presence of aflatoxins (AFs) and Ochratoxin A (OTA) contamination using high-performance liquid chromatography technique. The limit of detection and limit of quantification of AFs/OTA were 0.12/0.10 and 0.36/0.30 µg kg^?1, respectively. Only 5% of the samples were contaminated with AFs, ranging 0.15–2.58 µg kg^?1 with a mean of 0.05 ± 0.26 µg kg^?1. None of the raisin samples exhibited AFs contamination above the maximum limit (ML = 4 µg kg^?1) as set by the European Union (EU). About 72% of the samples were contaminated with OTA, ranging 0.14–12.75 µg kg^?1 with a mean of 2.10 ± 1.9 µg kg^?1. However, in 95.3% of the tested samples, OTA level was lower than the ML of 10 µg kg^?1 as regulated by the EU. Apparently, a strict and continuous monitoring plan, including regulatory limits, improves food safety and quality for all types of commodities.     

Determination of Polycyclic Aromatic Hydrocarbons (PAH4) in the Traditional Lebanese Grilled Chicken: Implementation of New,Rapid and Economic Analysis Method

Polycyclic aromatic hydrocarbons (PAH4) (benzo[a]anthracene, chrysene, benzo[b]fluoranthene, and benzo[a]pyrene) are evaluated in a traditional and widely consumed staple in Lebanon “Lebanese Grilled Chicken.” Forty samples with different local additives grilled by charcoal were purchased from different restaurants located in different regions in Lebanon. For this purpose, a simple and a reliable analytical method based on sonication technique and gas chromatography coupled to mass spectrometer (GC-MS) has been developed and validated. Several parameters affecting the extraction efficiency, such as the nature and the volume of the extract solvent, as well as other factors were investigated and optimized. The developed method is environmentally and economically friendly with a minimized consuming time, consisting of a single sonication step for 15 min using 12 mL of non-carcinogenic solvent acetonitrile (ACN) and without any further concentration prior to analysis. Following extraction, the cleanup step was based on freezing and d-SPE by C18 addition. Under optimized conditions, the method performances were evaluated; the limits of quantification (LOQs) achieved were lower than 0.689 μg kg^?1, and these values fit the performance criteria for the method given by the EC that defined the LOQ values of PAH lower than 0.9 μg kg^?1. In addition, the recovery values of the analyzed PAHs ranged from 88.9 to 119.3% with relative standard deviations (RSDs) less than 8% (n = 15). The levels of PAH4 were in the range from 1.52 to 49.9 μg kg^?1, where about 40% of the Lebanese grilled chicken exceeded the EU commission MRLs of 12 μg kg^?1.     

RP-HPLC-DAD Determination of Phenolics in Industrial Apple Pomace

Processing of apple fruits for juice/cider production generates large volume of pomace at industrial scale. This biomass (cell wall material and pulp tissues) is rich in array of nutrients, especially dietary fiber and polyphenols. Apple fruits confront various processing conditions at industrial level, influencing the biochemical composition of generated pomace, including its phenolic profile. In present study, a simple, fast and reproducible reversed-phase high-performance liquid chromatography method using diode array detector was developed and validated for separation of different phenolics present in industrial apple pomace. The present method showed reliable and reproducible intraday (0.2–4.0 % RSD) and interday (3.7–8.1 % RSD) precision with limits of detection and quantification values in range of 0.14–0.58 and 0.48–1.95 μg ml^?1, respectively, for all the phenolics. Different solvent-mediated extraction of dried pomace powder was also performed to evaluate its total antioxidant potential using standard spectrophotometric assays. The major phenolics found in industrial apple pomace extracts were quercetin (1.4–10.3 μg mg^?1), phloretin (1.1–9.3 μg mg^?1) and phloridzin (0.62–2.0 μg mg^?1).