Simultaneous extraction and determination of antibiotics in soils using a method based on quick,easy, cheap,effective, rugged,and safe extraction and liquid chromatography with tandem mass spectrometry

The increasing use of antibiotics has caused substantial environmental problems, which are a matter of great concern. The aim of this work was to develop a quick, easy, cheap, effective, rugged, and safe method for 20 antibiotic residues in soil. The developed method is based on extraction with acetonitrile and phosphate buffer, clean up with dispersive solid‐phase extraction adsorbent using primary secondary amine, octadecylsilane, followed by liquid chromatography with tandem mass spectrometry determination. We optimized different extraction methods and the ratio of cleanup adsorbents to achieve good recoveries at seven spiking levels that ranged from 61.4 to 118.9% with a relative standard deviation below 20% (n  = 5). The method quantification limit was in the range of 2–5 μg/kg for most analytes. Good linear regression coefficients greater than 0.990 were obtained. This method was applied for the analysis of real agricultural soil samples, confirming the feasibility of the method.     

Multiresidue analysis of 36 pesticides in soil using a modified quick,easy, cheap,effective, rugged,and safe method by liquid chromatography with tandem quadruple linear ion trap mass spectrometry

A new method for simultaneous determination of 36 pesticides, including 15 organophosphorus, six carbamate, and some other pesticides in soil was developed by liquid chromatography with tandem quadruple linear ion trap mass spectrometry. The extraction and clean‐up steps were optimized based on the quick, easy, cheap, effective, rugged, and safe method. The data were acquired in multiple reaction monitoring mode combined with enhanced product ion to increase confidence of the analytical results. Validation experiments were performed in soil samples. The average recoveries of pesticides at four spiking levels (1, 5, 50, and 100 μg/kg) ranged from 63 to 126% with relative standard deviation below 20%. The limits of detection of pesticides were 0.04–0.8 μg/kg, and the limits of quantification were 0.1–2.6 μg/kg. The correlation coefficients (r²) were higher than 0.990 in the linearity range of 0.5–200 μg/L for most of the pesticides. The method allowed for the analysis of the target pesticides in the lower μg/kg concentration range. The optimized method was then applied to the test of real soil samples obtained from several areas in China, confirming the feasibility of the method.     

Simultaneous determination of multiclass plant growth regulators in fruits using the quick,easy, cheap,effective, rugged,and safe method and ultra‐high performance liquid chromatography‐tandem mass spectrometry

In this study, a modified quick, easy, cheap, effective, rugged, and safe method combined with ultra‐high performance liquid chromatography and tandem mass spectrometry was developed for the multiclass determination of 28 plant growth regulators in various fruits. Different extraction solvents and adsorbents, including primary secondary amine, octadecylsilyl, graphitized carbon black, and zirconia‐based sorbent, were investigated. Internal calibration and isotope internal standards, chlormequat chloride‐d₄, mepiquat chloride‐d₆, indole‐3‐acetic acid‐d₂, and forchlorfenuron‐d₅ were used to improve accuracy. For method validation, good linearity, low limits of detection and quantification were obtained. At three spiked concentrations (10, 50, and 100 µg/kg), satisfactory recoveries with relative standard deviations of 2.4–17.5% were obtained for strawberries (75.2–119.8%), grapes (70.5–114.0%), tangerines (71.7–115.4%), apples (72.7–115.4%), and kiwi fruits (71.7–119.2%). Samples analysis revealed that 15.6% of the samples (n = 96) were contaminated with one or two kinds of plant growth regulators, including chlormequat chloride, forchlorfenuron, paclobutrazol, 2,4‐dichlorophenoxyacetic acid, 2‐diethylaminoethyl hexanoate, and mepiquat chloride. Similar results were obtained by ultra‐high performance liquid chromatography with quadrupole time‐of‐flight mass spectrometry, indicating the robustness, effectiveness, and suitability of the developed method for routine monitoring of plant growth regulator residues in fruits.     

Simultaneous determination of trifloxystrobin and trifloxystrobin acid residue in rice and soil by a modified quick,easy, cheap,effective, rugged,and safe method using ultra high performance liquid chromatography with tandem mass spectrometry

A sensitive analytical method for the simultaneous determination of trifloxystrobin and its metabolite trifloxystrobin acid in rice including straw, bran, brown rice and soil was developed by using ultra high performance liquid chromatography coupled with tandem mass spectrometry. The fungicide trifloxystrobin and its metabolite trifloxystrobin acid were extracted using acetonitrile with 1% formic acid v/v and subsequently cleaned up by primary secondary amine, octadecylsilane or graphitized carbon black prior to ultra high performance liquid chromatography coupled with tandem mass spectrometry. The determination of two target compounds was achieved in less than 3 min using an electrospray ionization source in positive mode. The limits of detection were below 0.22 μg/kg and the limits of quantification did not exceed 0.74 μg/kg in all matrices, which were much lower than the maximum residue levels established by the Codex Alimentarius Commission. The overall average recoveries in four matrix at three levels (0.1, 1.0 and 5.0 mg/kg) ranged from 74.2 to 107.4% with a relative standard deviations of less than 7.8% (n = 5) for both analytes. The method was demonstrated to be convenient and reliable for the routine monitoring of trifloxystrobin and its metabolite. The developed method was validated and applied for the analysis of degradation study samples.     

A quick,easy, cheap,effective, rugged,and safe method for the simultaneous detection of four triazolone herbicides in cereals combined with ultrahigh performance liquid chromatography with tandem mass spectrometry

This paper describes a novel, rapid, and sensitive analytical method for monitoring four triazolone herbicides in cereals (wheat, rice, corn, and soybean), using a quick, easy, cheap, effective, rugged, and safe sample extraction procedure followed by ultrahigh performance liquid chromatography coupled with tandem mass spectrometry. The four triazolone herbicides (amicarbazone, carfentrazone‐ethyl, sulfentrazone, and thiencarbazone‐methyl) were extracted using acidified acetonitrile (containing 1% v/v formic acid) and subsequently purified with octadecylsilane (C₁₈) prior to sample analysis. Ultrahigh performance liquid chromatography coupled with tandem mass spectrometry was operated in positive and negative ionization switching mode. Amicarbazone and carfentrazone‐ethyl were detected in the positive mode (ESI+), while sulfentrazone and thiencarbazone‐methyl were detected in the negative mode (ESI?). All compounds were successfully separated in less than 3.0 min. Further optimization achieved desired recoveries ranging from 74.5 to 102.1% for all analytes with relative standard deviation values ≤17.2% in all tested matrices at three levels (10, 100, and 500 μg/kg). The limits of detection for all compounds were ≤2.3 μg/kg, and the limits of quantitation did not exceed 7.1 μg/kg. The developed method showed excellent linearity (R² ≥ 0.994) and was proven to be highly efficient and reliable for the routine monitoring of triazolone herbicides in cereals.     

Comparison of extraction solvents and sorbents in the quick,easy, cheap,effective, rugged,and safe method for the determination of pesticide multiresidue in fruits by ultra high performance liquid chromatography with tandem mass spectrometry

An improved analytical method was developed for the simultaneous quantification of several plant growth regulators and fungicides (carbendazim, pyrimethanil, metalaxyl, triadimefon, paclobutrazol, thiophanate, prochloraz, dimethomorph, difenoconazole, (4‐chlorophenoxy)‐acetic acid, (2,4‐dichlorophenoxy)‐acetic acid, thiadiazuron, forchlorfenuron and gibberellins) in fruits followed by ultra high performance liquid chromatography with tandem mass spectrometry. Samples were extracted and purified using a modified QuEChERS method. Different extraction solvents and sorbents in the QuEChERS method were compared. Optimum results were followed by the addition of 1% acetic acid in acetonitrile; C₁₈ sorbent was added due to the acidic nature of several pesticides. The recoveries of the pesticides were in the range 73.7–118.4%, with relative standard deviations lower than 16.63%. Limits of detection ranged from 0.1–1.0 μg/kg. The method presented here is simple, rapid, sensitive and can be applied to large‐scale monitoring programs to screen the presences of pesticides in fruits.     

Determination of hexabromocyclododecane enantiomers in chicken whole blood by a modified quick,easy, cheap,effective, rugged,and safe method with liquid chromatography and tandem mass spectrometry

A rapid and simple analytical method has been developed for the determination of hexabromocyclododecane enantiomers in chicken whole blood, based on a modified quick, easy, cheap, effective, rugged, and safe approach before liquid chromatography coupled with tandem mass spectrometry. The factors influencing performance of method were investigated by single factor experiment, and further optimized by the response surface methodology based on Box–Behnken design. The matrix effects were also evaluated by the isotopic dilution method. Under the optimal conditions, the proposed method showed good linearity within the range of 1–500 μg/L and good repeatability with relative standard deviation less than 9.5% (n = 5). The limits of detection (S/N = 3) were 0.03–0.19 μg/L. The developed method was successfully applied for the analysis of hexabromocyclododecane enantiomers in real chicken blood samples. The satisfactory recoveries ranging of 83.6–115.0% were obtained (at spiked levels of 5, 20, and 100 μg/L). The results demonstrated that the proposed method would be a practical value method for the determination of hexabromocyclododecane enantiomers in animal blood. It would be further developed with confidence to analyze other lipophilic organic pollutants in blood sample.     

Simultaneous determination of flupyradifurone and its two metabolites in fruits,vegetables, and grains by a modified quick,easy, cheap,effective, rugged,and safe method using ultra high performance liquid chromatography with tandem mass spectrometry

An effective analytical method for the simultaneous determination of a novel insecticide flupyradifurone and its two metabolites was developed using ultra high performance liquid chromatography with tandem mass spectrometry coupled with a quick, easy, cheap, effective, rugged, and safe procedure. The three target compounds were extracted with acetonitrile and cleaned up with octadecylsilane, and were separated successfully between 1.9 and 3.1 min using an HSS T3 chromatographic column connected to an electrospray ionization source. All the matrix‐matched samples at three fortified levels (0.01, 0.05, and 0.5 mg/kg) provided satisfactory recoveries in the range of 70.3–116.5% with relative standard deviations below 18.6%. The limits of quantitation were 10 μg/kg for flupyradifurone and difluoroethylamino‐furanone and 100 μg/kg for 6‐chloronicotinic acid. The limit of quantification of flupyradifurone was far below the maximum residue limit in the USA. The method is of great significance for establishing maximum residue limits in China.     

A quick,easy, cheap,effective, rugged,and safe sample pretreatment and liquid chromatography with tandem mass spectrometry method for the simultaneous quantification of 33 mycotoxins in Lentinula edodes

Lentinula edodes, one of the most cultivated edible fungi in the world, are usually neglected for mycotoxins contamination due to the initial thinking of its resistance to mycotoxingenic molds. In the present study, a sensitive and reliable liquid chromatography with tandem mass spectrometry method was developed for the simultaneous quantification of 33 mycotoxins in L. edodes. Targeted mycotoxins were extracted using a quick, easy, cheap, effective, rugged, and safe procedure without any further clean‐up step, and analyzed by liquid chromatography with tandem mass spectrometry on an Agilent Poroshell 120 EC‐C₁₈ column (100 × 3 mm, 2.7 μm) with a linear gradient elution program using water containing 5 mM ammonium acetate and methanol as the mobile phase. After validation by determining linearity (R² > 0.99), sensitivity (LOQ ≤ 20 ng/kg), recovery (73.6–117.9%), and precision (0.8–19.5%), the established method has been successfully applied to reveal the contamination states of various mycotoxins in L. edodes. Among the 30 tested samples, 22 were contaminated by various mycotoxins with the concentration levels ranging from 3.3–28 850.7 μg/kg, predicting that the edible fungus could be infected by the mycotoxins‐producing fungi. To the best of our knowledge, this is the first report about real mycotoxins contamination in L. edodes.     

Simultaneous determination of three herbicides in wheat,wheat straw,and soil using a quick,easy, cheap,effective, rugged,and safe method with ultra high performance liquid chromatography and tandem mass spectrometry

In this study, a sensitive and effective analytical method for the extraction and detection of three herbicide residues (florasulam, fluroxypyr, and halauxifen‐methyl) in wheat and soil was developed. Samples were extracted with acetonitrile/water followed by salting out, dispersive solid‐phase extraction cleanup, and detection using ultra high performance liquid chromatography coupled with tandem mass spectrometry. The target analytes were detected within a 5 min runtime using an ultra high performance liquid chromatography high‐strength silica trifunctional column connected to an electrospray ionization source in positive mode. The method was validated in five replicates at three fortification concentrations in each matrix. Adequate pesticide quantification and identity confirmation were attained, even at the lowest concentration levels. The method showed very good accuracy and precision. Good recoveries were observed for the three herbicides and mostly ranged between 75.8 and 114.6%, with intraday relative standard deviations <6.01% and interday relative standard deviations <4.02%. The limits of quantification ranged between 0.14 and 7.68 μg/kg for each herbicide. The method was successfully applied for the simultaneous analysis of the three herbicides in actual trial samples, and the results proved that the proposed method was effective in detecting these three herbicides.     

Determination of cyflumetofen residue in water,soil, and fruits by modified quick,easy, cheap,effective, rugged,and safe method coupled to gas chromatography/tandem mass spectrometry

A new, highly sensitive, and selective method was developed for the determination of the cyflumetofen residue in water, soil, and fruits by using gas chromatography quadruple mass spectrometry. The target compound was extracted using acetonitrile and then cleaned up using dispersive solid‐phase extraction with primary and secondary amine and graphitized carbon black, and optionally by a freezing‐out cleanup step. The matrix‐matched standards gave satisfactory recoveries and relative standard deviation values in different matrices at three fortified levels (0.05, 0.5, and 1.0 mg kg^?1). The overall average recoveries for this method in water, soil, and all fruits matrix at three fortified levels ranged from 76.3 to 101.5% with relative standard deviations in the range of 1.2–11.8% (n = 5). The calculated limits of detection and quantification were typically below 0.005 and 0.015 μg kg^?1, which were much lower than the maximum residue levels established by Japanese Positive List. This study provides a theoretical basis for China to draw up maximum residue level and analytical method for cyflumetofen acaricide in different fruits.     

Determination of multiple antibiotics in agricultural soil using a quick,easy, cheap,effective, rugged,and safe method coupled with ultra-high performance liquid chromatography-tandem mass spectrometry

In this study, we combined ultra-high performance liquid chromatography with tandem mass spectrometry to establish a quick, easy, cheap, effective, rugged, and safe method of detecting 21 target antibiotics in agricultural soil samples. Antibiotics were extracted with mixed solvents consisting of ethylenediaminetetraacetic acid disodium salt dihydrate and phosphoric acid citric acid buffer and acetonitrile which were purified with octadecylsilyl as an adsorbent and anhydrous sodium sulfate as a desiccant. This method was able to effectively extract all of the target antibiotics from agricultural soils, with recovery efficiencies ranging from 55 to 108% and limits of detection between 0.09–0.68 μg/kg. We also validated this new method for selectivity, sensitivity, and reliability of detecting multiple antibiotics in 12 samples. Considering the potential environmental and public health effects of antibiotics in agricultural soils, our new method can help analyze the degree of antibiotic contamination and provide valuable information for soil quality and risk assessment.     

Simultaneous determination of antiviral drugs in chicken tissues by ultra high performance liquid chromatography with tandem mass spectrometry

An ultra high performance liquid chromatography with tandem mass spectrometry method was established for the rapid and simultaneous analysis of seven antiviral drugs, amantadine, rimantadine, memantine, moroxydine, imiquimod, oseltamivir, and acyclovir, in chicken liver, muscle, and egg. Homogenized samples were extracted with trichloroacetic acid and acetonitrile solutions and then purified by cation‐exchange solid‐phase extraction. The target drugs were analyzed by liquid chromatography with a UPLC BEH Amide column (2.1 mm × 100 mm, 1.7 μm) coupled with a tandem mass spectrometer operating in the positive multiple‐reaction mode. A perfectly linear relationship was obtained within the concentration ranges of 0.5–20 μg/L for acyclovir and 0.1–10 μg/L for the other six antiviral drugs. The average recoveries of the seven antiviral drugs using four addition levels in chicken liver, muscle, and eggs were 82.67–90.10, 82.30–92.27, and 81.98–93.77%, respectively, and the acceptable coefficients of variation were 5.18–9.88, 4.84–11.2, and 42.8–9.95%, respectively. The detection limits and detection capabilities of the analysis method for the seven antiviral drugs were in the ranges of 0.04–0.64 and 0.11–0.78 μg/kg, respectively. Additionally, an inter‐laboratory study among five laboratories further validated the method.     

Qualitative-quantitative analysis of multi-mycotoxin in milk using the high-performance liquid chromatography-tandem mass spectrometry coupled with the quick,easy, cheap,effective, rugged and safe method

High-performance liquid chromatography-tandem mass spectrometry coupled with the quick, easy, cheap, effective, rugged and safe method was established for the qualitative and quantitative detections of 20 mycotoxins in milk. The linear range of this method was 0.01–10 μg/L and the correlation coefficients were all greater than or equal to 0.9933. At three levels of addition, the spiked recoveries ranged from 80.00 to 112.50%, relative standard deviations were 2.67–14.97%, limits of quantitation were 0.02–4.00 μg/kg, and limits of detection were 0.007–1.300 μg/kg. This developed procedure for the identification and quantitation of mycotoxins provided prospective support for quality regulation.     

Enantioselective determination of triazole fungicide simeconazole in vegetables, fruits, and cereals using modified QuEChERS (quick, easy, cheap, effective, rugged and safe) coupled to gas chromatography/tandem mass spectrometry

A rapid and effective method for enantioselective determination of simeconazole enantiomers in food products (cucumber, tomato, apple, pear, wheat and rice) has been developed. The enantiomers were resolved by capillary gas chromatography (GC) using a commercial chiral column (BGB-172) and a temperature program from 150 °C (held for 1 min) and then raised at 10 °C min⁻¹ to 240 °C (held for 10 min). This enantioselective gas chromatographic separation was combined with a clean-up/enrichment procedure based on the modification of QuEChERS (quick, easy, cheap, effective, rugged and safe) method. Co-extractives were removed with graphitized carbon black/primary secondary amine (GCB/PSA) solid-phase extraction (SPE) cartridges using acetonitrile:toluene (3:1, v/v) as eluent. Gas chromatography/ion trap mass spectrometry (GC–ITMS) with electron ionization (EI) was then used for qualitative and quantitative determination of the simeconazole enantiomers. Two precursor-to-product ion transitions (m/z 121–101 and 195–153) with the best signal intensity were chosen to build the multiple-reaction monitoring (MRM) acquisition method. The limits of detection for each enantiomer of simeconazole in six food products ranged between 0.4 and 0.9 μg kg⁻¹, which were much lower than maximum residue levels (MRLs) established by Japan. The methodology was successfully applied for the enantioselective analysis of simeconazole enantiomers in real samples, indicating its efficacy in investigating the environmental stereochemistry of simeconazole in food matrix.     

Rapid residue analysis of oxathiapiprolin and its metabolites in typical Chinese soil,water, and sediments by a modified quick,easy, cheap,effective, rugged,and safe method with ultra high performance liquid chromatography and tandem mass spectrometry

A sensitive and effective method for the simultaneous determination of residues from a new fungicide, oxathiapiprolin, and its metabolites (IN‐E8S72 and IN‐WR791) in soil, water, and sediment, was developed using ultra high performance liquid chromatography with tandem mass spectrometry. Three compounds were extracted from water, soil, and sediment by using acetonitrile and different proportions of formic acid aqueous solution (1% v/v for water; 2% v/v for soil; and sediment), and were cleaned with octadecylsilane. The target compounds were determined within 5 min using an electrospray ionization source in the positive mode for oxathiapiprolin and in the negative mode for the two metabolites. The limits of quantification for all the three compounds were 0.1 μg/kg in water and 1 μg/kg in soil and sediment. Recovery studies were performed using three spiked levels (0.1, 1, and 10 μg/kg for water; 1, 10, and 50 μg/kg for soil and sediment). The overall average recoveries ranged from 64.8 to 112.7% with all intra‐ and interday relative standard deviation values below 19.4 and 19.1%, respectively. The method validation confirmed that the proposed method was convenient and reliable for determining residual oxathiapiprolin and its metabolites in soil, water, and sediments.     

Innovative mixture of salts in the quick,easy, cheap,effective, rugged,and safe method for the extraction of residual macrolides in milk followed by analysis with liquid chromatography and tandem mass spectrometry

A simple extraction technique has been developed for seven macrolide antibiotics in milk. The procedure involves a modified quick, easy, cheap, effective, rugged, and safe method based on acetonitrile extraction, followed by the addition of a mixture of salts (sodium sulfate, sodium chloride, and potassium carbonate) not yet reported in literature. The method was validated for tylosin and was selective, free of matrix effect, and linear in the range of 0.78–18.75 ng/mL in the final extract, corresponding to 0.125–3 times the maximum residue limit. The limit of detection, limit of quantification, decision limit, and detection capability were, respectively, 0.84, 2.79, 58.4, and 71.7 μg/kg. The overall average recovery at 25, 50, and 75 μg/kg ranged from 89–97%. Repeatability and intermediate precision expressed by relative standard deviations were below 10.5 and 12%, respectively. The extension of the validation for spiramycin, throleandomycin, oleandomycin, roxithromycin, erythromycin, and clarithromycin is under consideration since the procedure proved to be able to efficiently extract all studied macrolides, with recoveries from 74–104% at 50 μg/kg for tylosin, erythromycin, spiramycin, and oleandomycin and 20 μg/kg for throleandomycin, roxithromycin, and clarithromycin.     

Simultaneous determination of pesticides, biopesticides and mycotoxins in organic products applying a quick, easy, cheap, effective, rugged and safe extraction procedure and ultra-high performance liquid chromatography-tandem mass spectrometry

A method for the simultaneous determination of pesticides, biopesticides and mycotoxins from organic products was developed. Extraction of more than 90 compounds was evaluated and performed by using a modified QuEChERS-based (acronym of Quick, Easy, Cheap, Effective, Rugged, and Safe) sample preparation procedure. The method was based on a single extraction with acidified acetonitrile, followed by partitioning with salts, avoiding any clean-up step prior the determination by ultra-high performance liquid chromatography/tandem quadrupole mass spectrometry (UHPLC–MS/MS). Validation studies were carried out in wheat, cucumber and red wine as representative matrixes. Recoveries of the spiked samples were in the range between 70 and 120% (with intra-day precision, expressed as relative standard deviation, lower than 20%) for most of the analysed compounds, except picloram and quinmerac. Inter-day precision, expressed as relative standard deviation, was lower than 24%. Limits of quantification were lower than 10 μg kg⁻¹ and the developed method was successfully applied to the analysis of organic food products, detecting analytes belonging to the three types of compounds.     

Ethanol-ammonium sulfate system based modified quick,easy, cheap,effective, rugged,and safe method for the determination of four neonicotinoid pesticide and metabolite residues in two canned fruits

As the pesticide and its metabolite residues in processed fruits could become a significant route of human exposure. The work presented herein focuses on developing a feasible quick, easy, cheap, effective, rugged, and safe method with improved extraction and cleanup system for the determination of imidacloprid, acetamiprid, thiamethoxam, and clothianidin (a metabolite of thiamethoxam) in canned fruits. The low toxic solvent ethanol was used to extract the analytes, and ammonium sulfate was used to promote phase separation. Moreover, the carboxylated multi-walled carbon nanotube acted as the clean-up sorbent for the removal of high solubility impurities. The proposed method was validated with fortified real samples at different concentration levels (20–200 μg/kg). Recoveries obtained from three spiked levels (20, 50, and 200 μg/kg) ranged from 74.9 to 86.4% with relative standard deviations of the intra-day and inter-day in the range of 0.8–5.5 and 2.0–7.1%, respectively. The limits of detection ranged from 0.2 to 0.5 and 0.2 to 0.6 μg/kg for orange and peach, respectively. The results demonstrated that the proposed method could be considered appropriate, and comparatively lower toxic for the analysis of neonicotinoid pesticide residues in canned fruit.     

Multi-residue analysis of 206 pesticides in grass forage by the one-step quick,easy, cheap,effective, rugged,and safe method combined with ultrahigh-performance liquid chromatography quadrupole orbitrap mass spectrometry

A novel method for detecting pesticide multi-residue in grass forage (alfalfa and oat) was established based on the one-step automatic extraction and purification technology of quick, easy, cheap, effective, rugged, and safe combined with ultrahigh-performance liquid chromatography quadrupole Orbitrap high-resolution mass spectrometry. The crushed sample was extracted with acetonitrile with 1% acetate, followed by a cleanup step with a primary-secondary amine, octadecylsilane, and graphitized carbon black. The extraction and purification were carried out using the one-step automatic pretreatment equipment. The target pesticides were acquired in positive ion electrospray ionization mode and full scan/data dependent secondary scan mode. The calibration curve shows good linearity over the corresponding concentration range, with the coefficient of determination greater than 0.99. The screening detection limits were 0.5–50 μg/kg, and the limit of quantification for the 206 pesticides was set at 1–50 μg/kg. At the spiking levels of one, two, and 10 times of limit of quantification, more than 95% of pesticides had recovery between 70–120%, with a relative standard deviation ≤20%. The method was proved to be simple, rapid, high-sensitivity, and could be routinely used for the high throughput screening and quantitative analysis of pesticide residues in alfalfa and oat.