Multiplug Filtration Cleanup Research Articles

Accurate and stable detection of p-phenylenediamine antioxidants and their transformation products in aquatic products using antioxidant protection – Analysis of actual aquatic products

Given the high toxicity of N-(1,3-dimethylbutyl)-N′-phenyl-p-phenylenediamine (6PPD) derivatives, such as 6PPD quinone (6PPDQ) to salmon, as well as their ubiquitous presence in the environment, the contaminant of aquatic food products has drawn significant attention. However, analytical methods for p-Phenylenediamines (PPDs) and their transformation products (TPs) in aquatic products remain underdeveloped. In particular, the degradation of some compounds and strong matrix effects complicate detection. In this study, we present a stable, rapid, and sensitive method combining salt-out assisted extraction, antioxidant protection, and multi-plug filtration clean-up (m-PFC) to detect two PPDs and five TPs in aquatic products. Crucially, the appropriate selection of antioxidants prevented the degradation of the easily oxidized target compounds. Further, the m-PFC method significantly enhanced the purification efficiency, achieving satisfactory recoveries (62.1–115 %), and method detection limits (MDLs) ranging from 0.00300 to 0.400 μg/kg. Subsequently, the method was applied to monitor PPDs and their TPs in aquatic products systematically, revealing the presence of 6PPD and N-isopropyl-N′-phenyl-1,4-phenylenediamine (IPPD) in white shrimp from aquafarms, whereas none of the seven target analytes were detected in fish and crab samples. These findings contribute to the detection of PPDs, their TPs and other unstable chemicals in aquatic products, thereby providing insights into their concentrations in these products.

A comparison of the determination of multiple pesticide residues in fruits, vegetables, and edible fungi using gas chromatography combined with filtration purification and solid-phase extraction.

The multiplug filtration clean-up (m-PFC) and solid-phase extraction (SPE) pretreatment methods were employed to process 8 representative matrices in fruits, vegetables, and edible fungi, respectively. 37 pesticide residues were determined using gas chromatography equipped with ECD and FPD detectors. The measurement data were compared and analyzed following m-PFC purification and gas chromatography analysis, and both accuracy and precision met the (EU) 2021/808 requirements, achieving recovery rates for the 8 matrices ranging from 67.0% to 112.8% (averaging over 83.8% recovery), and RSDs between 0.2% and 15.2%. The 37 pesticides exhibited good linearity between 0.05 and 1.6 μg mL-1, and the matrix effect was found to be weaker compared to that of the Florisil solid-phase extraction method. The detection limits ranged from 0.0001 to 0.03 μg kg-1, with 31 pesticides showing lower detection limits compared to the SPE method. The application of this method to 150 real samples resulted in the detection of 17 pesticides across all samples. Fewer pigments were detected in m-PFC purified solutions compared to Florisil PR SPE when analyzed by liquid chromatography. m-PFC achieved more thorough adsorption of endogenous substances like pigments, reducing instrument contamination, utilizing less organic solvent, and simplifying the operation. This purification step offers clear advantages, allowing for the processing of larger sample batches in a short time. It can serve as a replacement for SPE methods like Florisi PR in batch detection of fruit and vegetable samples.

Determination of 14 perfluoroalkyl substances in Chinese mitten crab by multi-plug filtration cleanup coupled with ultra-performance liquid chromatography-tandem mass spectrometry

Determination of 14 perfluoroalkyl substances in Chinese mitten crab by multi-plug filtration cleanup coupled with ultra-performance liquid chromatography-tandem mass spectrometry

Residue Levels and Dietary Intake Risk Assessments of 139 Pesticides in Agricultural Produce Using the m-PFC Method Based on SBA-15-C18 with GC-MS/MS.

A survey was designed to investigate the pesticide residues in agricultural produce and to estimate their potential intake risks to inhabitants. A total of 314 samples of nine types of fruits and vegetables were collected from the supermarkets and vegetable markets of Shandong Province (China) from October 2020 to February 2022. An accurate and reliable multi-residue method, based on GC-MS/MS detection, as well as the multiplug filtration cleanup method, based on SBA-15-C18, was prepared by a solution chemical reaction. Additionally, an in situ co-condensation method was established for the quantification of 139 pesticide residues. Residues that contained no pesticides were detected in 66.5% of the 314 samples. Moreover, of the samples, 30.6% were at or below the MRLs, and 2.9% were above the MRLs. Residues of procymidone were found to be the one that most often exceeded the MRLs (1.3% of the samples). Tebuconazole was found most frequently in 22.0% of the samples analyzed. Consumer exposure to the 139 pesticides did not exceed 100% ADI and ARfD. This led to a consideration that these pesticide residues in the nine commodities may not raise the health risk of the consumers in the long and short term. The highest value of chronic dietary intake was obtained from spirodiclofen, which resulted in a 24.1% of ADI. Furthermore, the highest exposure levels in the short term were obtained from the consumption of leeks with procymidone (58.3% ARfD).

Determination of Multi-pesticides Residues in Jasmine Flower and Its Scented Tea.

For minor crops such as jasmine, the lack of pesticide registration and maximum residue limits are important issues that need to be solved in order to facilitate trading and ensure food safety. Meanwhile, reliable and quick analytical methods for multi-pesticide residues in these commodities are few, but required by various stakeholders. In this study, a method for detecting twenty-five most frequently used pesticides in jasmine flower and its scented tea by multi-plug filtration cleanup and ultra-high-performance liquid chromatography-tandem mass spectrometry was developed and validated. The cleanup process was optimized and compared with the dispersive solid phase extraction procedure. The method was validated, showing that except for methomyl, recoveries of twenty-five pesticides were 64%-108%, with relative standard deviations (n = 5) of 0.33%-10%. The method was successfully applied to detect pesticide residues in marketed samples. The results showed that some flower and tea samples contained a combination of different pesticide residues.

Automatic Multi-Plug Filtration Cleanup Tip-Filtration with Ultra-Performance Liquid Chromatography/Tandem Mass Spectrometry Detection For 22 Pesticide Residues in Typical Vegetables.

An automatic multi-plug filtration cleanup (m-PFC) tip-filtration method was developed to reduce the manual operation workload in sample preparation. In this work, m-PFC was based on multi-walled carbon nanotubes mixed with primary secondary amines and anhydrous magnesium sulfate (MgSO4) in a packed column for analysis of pesticide residues followed by ultra-performance liquid chromatography coupled with tandem mass spectrometry. Method validation was performed on 22 pesticide residues in carrot, spinach and leek, at spiked levels of 5, 10 and 50μg/kg, respectively. The average recoveries were between 70.1 and 119.5% with associated relative standard deviations <20% (n = 6) indicating satisfactory accuracy and repeatability. Matrix-matched calibration curves were performed with the correlation coefficients (R2) higher than 0.9903 within a linearity range of 5-100ng/mL. The limits of quantification were 5μg/kg for all the pesticides in carrot, spinach and leek matrices. The developed method was successfully used to determine pesticide residues in market samples.

Automated multi-plug filtration cleanup method for analysis of 48 pesticide residues in green tea using liquid chromatography-tandem mass spectrometry

An automated multi-plug filtration cleanup (m-PFC) method, based on QuEChERS extraction was developed for the analysis of 48 pesticides in green tea. The carboxyl functionalized multi-walled carbon nanotubes (MWCNTs-COOH) were firstly packed in m-PFC columns and functioned as promising sorbents with better clean-up capability. The different parameters of automated m-PFC equipment and extraction conditions were optimized. The automated method integrated cleanup and filtration (through filter membrane) procedure into a single run before injected to the detection instrument. Comparison to d-SPE and manual m-PFC method, the automated method could handle a batch of samples simultaneously with better purification effect. Acceptable recoveries at three concentration levels from 71% to 114% were obtained (except carbendazim and bifenazate) with relative standard deviations lower than 18%. The proposed automated m-PFC method offered a great compromise between rapidity, convenience and efficiency. It was successfully applied for market monitoring of pesticide residues with robust analyze data. • Automated m-PFC method for analysis of 48 pesticides in green tea. • Functionalized MWCNTs were mixed with other sorbents to assess cleanup performance. • Extraction and automated m-PFC process were optimized by recovery and matrix effect. • Method validation showed superior purification efficiency and robust analysis data. • The automated method can handle a batch of real sample in routine pesticide analysis.

A multi-plug filtration (m-PFC) cleanup method based on carboxylic multi-walled carbon nanotubes for the detection of 14 perfluorinated compounds and dietary risk assessment of chicken, beef, and mutton collected from Shanghai markets

Dietary intake is a major pathway of human exposure to perfluorinated compounds (PFCs). Livestock and poultry meats (chicken, beef, mutton) account for a significant proportion of dietary consumption in China, and thus it is crucial to investigate the levels and composition profiles of PFCs in consumer meats to assess and mitigate potential health risks. However, rapid and simple analytical methods for such investigations are lacking. This study addresses this shortcoming by developing a rapid filtration clean-up method using carboxylic multi-walled carbon nanotubes (CMWCNTs) for the detection of 14 PFCs. Good linearities (R2 > 0.99) were obtained for all 14 PFCs in chicken, beef, and mutton. Recoveries ranged from 65 to 145% (except perfluorotetradecanoic acid, PFTeDA) with relative standard deviations (RSDs) lower than 16%. Method limits of detection (LODs) were between 0.12 and 0.83 ng g−1d.w. Subsequently, this method was applied for the analysis of 46 livestock and poultry meat samples collected from markets in Shanghai. PFCs were detected in all samples with total concentrations of 1.61–4.27 ng g−1 wet weight (w.w) in chicken, 1.51–5.56 ng g−1 w.w in beef and 1.61–8.15 ng g−1 w.w in mutton. Perfluorooctanoic acid (PFOA) and perfluorobutanoic acid (PFBA) were the predominant compounds in these samples and accounted for over 92% of ΣPFCs. For regulated compounds such as PFOA, risk quotients (RQs) were determined to be much lower than 1. This suggests that chicken, beef, and mutton from Shanghai market pose very low PFC exposure risk to residents. However, high detection frequency of the unregulated PFBA demands further investigation of short-chain PFCs in consumer meats.

Utilizing a Rapid Multi-Plug Filtration Cleanup Method for 72 Pesticide Residues in Grape Wines Followed by Detection with Gas Chromatography Tandem Mass Spectrometry

A convenient and fast multi-residue method for the efficient identification and quantification of 72 pesticides belonging to different chemical classes in red and white grape wines has been developed. The analysis was based on gas chromatography tandem quadrupole mass spectrometric determination (GC–MS/MS). The optimization strategy involved the selection of the amount of multi-walled carbon nanotubes (MWCNTs) and the number of cleanup procedure cycles for multi-plug filtration cleanup (m-PFC) to achieve ideal recoveries and reduce the sample matrix compounds in the final extracts. The optimized procedure obtained consistent recoveries between 70.2 and 108.8% (70.2 and 108.8% for white wine, and 72.3 and 108.4% for red wine), with relative standard deviations (RSDs) that were generally lower than 9.2% at the three spiking levels of 0.01, 0.05 and 0.1 mg/kg. The linearity was studied in the range between 0.002 and 0.1 mg/kg using pesticide standards prepared both in pure solvent and in the presence of the matrix, showing coefficients of determination (R2) higher than 0.9495 for all the pesticides. To improve accuracy, matrix-matched calibration curves were used for calculating the quantification results. Finally, the method was used successfully for detecting pesticide residues in commercial grape wines.

Determination of Six Eugenol Residues in Aquatic Products by Gas Chromatography-Orbitrap Mass Spectrometry

Eugenol compounds are widely used in the circulation and transportation of fresh aquatic products because of their good anesthetic effects. However, some studies have shown that eugenol compounds are potential carcinogens. Therefore, in order to ensure the edible safety of aquatic products, eugenol compounds in aquatic products need to be screened quickly. A method for determination of six eugenol residues in aquatic products was established by multiplug filtration cleanup (m-PFC), combined with gas chromatography-Orbitrap mass spectrometry (Orbitrap GC-MS). Samples were ultrasonically extracted with acetonitrile, and the extracts were frozen at −18°C for 1 h, then purified with the m-PFC column, and detected by Orbitrap GC-MS in full scan mode. The results showed the linear relationships for six eugenols were good in the range of 0.001–0.1 μg/mL, and the correlation coefficients (R2) were above 0.9950. The limits of detection (LODs) were 2–10 μg/kg, and the limits of quantitation (LOQs) were 5–20 μg/kg. The average recoveries at the spiked levels of 5–200 μg/kg were in the range of 76.4%–105.1%, with relative standard deviations (RSDs) of 1.2%–7.5%. Eighty aquatic products were detected by this method, of which only eugenol was detected in 12 samples, and eugenol and isoeugenol were detected in two samples at the same time. The other eugenol compounds were not detected in any sample. The detection rate of positive samples was 17.5%. The method is simple, accurate, and suitable for the rapid screening of eugenol compounds in aquatic products.

Rapid Screening of 350 Pesticide Residues in Vegetable and Fruit Juices by Multi-Plug Filtration Cleanup Method Combined with Gas Chromatography-Electrostatic Field Orbitrap High Resolution Mass Spectrometry.

A new method for screening pesticide residues in vegetable and fruit juices by the multi-plug filtration cleanup (m-PFC) method combined with gas chromatography-electrostatic field orbitrap high resolution mass spectrometry(GC-Orbitrap/MS) was developed. The samples were extracted with acetonitrile, purified with m-PFC and determined by GC-Orbitrap/MS. Qualitative analysis was confirmed by retention time, accurate molecular mass and quantitative analysis were performed with the matrix standard calibration. It could eliminate matrix interference effectively. Eight kinds of typical samples (orange juice, apple juice, grape juice, strawberry juice, celery juice, carrot juice, cucumber juice, tomato juice) were evaluated. The linear ranges of the 350 pesticides were from 5 to 500 μg/kg, with good correlation coefficients greater than 0.990. The limits of detection (LODs) were 0.3–3.0 μg/kg and the limits of quantification (LOQs) were 1.0–10.0 μg/kg. The average recoveries at three spiked levels of 10, 100, 200 μg/kg were in the range of 72.8–122.4%, with relative standard deviations (RSDs) of 2.0–10.8%. The method has effectively improved the determination efficiency of pesticide residue screening by high-resolution mass spectrometry in vegetable and fruit juices.

Detect 15 pesticides fungicide in edible fungi by multiplug filtration clean-up pretreatment technology with ultra-high performance liquid chromatography-tandem mass spectrometry

To establish a method for determination of 15 pesticides residue in edible fungi by multiplug filtration clean-up(m-PFC) pretreatment technique with ultra-high performance liquid chromatography-tandem triple quadruple mass spectrometry(UPLC-MS/MS). The interferences of edible fungus samples were removed by extracting with acetonitrile and filtration type extraction column, which were fat, carbohydrates, water-soluble vitamins. Samples were separated with column of Waters ACQUITY UPLC®HSS T3(2.1 mm×100 mm, 1.8 μm), and were scanned by multiple reaction monitoring mode(MRM). Samples were quantified with matrix matching standard curve external standard method. The recoveries of 15 target compounds at the spiked levels of 10, 20, 50 μg/kg were 82.5%-118.5%, and the relative standard deviations were between 6.1% and 23.1%(n=6). The detection limit of 15 target compounds was 1-3 μg/kg, and the limit of quantification was 3-10 μg/kg. This method improves the efficiency of pretreatment, has good stability and high sensitivity, and could be used for the detection of 15 pesticides in edible fungi.

Simultaneous determination of 14 pesticide residues in tea by multi-plug filtration cleanup combined with LC-MS/MS

A combined method of multi-plug filtration cleanup (m-PFC) and liquid chromatography-triple quadrupole mass spectrometry (LC-MS/MS) was established to simultaneously detect 14 pesticides in tea. The pesticides in water-soaked tea were extracted with acetonitrile. Cleanup of tea extract was performed using an m-PFC column packed with multiple cleanup materials: multi-walled carbon nano-tubes (MWCNTs), primary secondary amine (PSA) and anhydrous magnesium sulfate (MgSO4). The cleanup effect of the column was evaluated based on the rates of removal of tea components that interfered with pesticide recovery, henceforth referred to as interference components. Results showed that 14 pesticides had strong linearity in the range of 5–500 μg L−1 (r2 > 0.99). The quantitative limits were within the range of 3–50 μg kg−1. The average recoveries of 14 pesticides spiked into three different blank tea samples (green tea, black tea, oolong tea) at three levels of 0.05, 0.50 and 2.00 mg kg−1 were in the range of 62.3–108.8% with relative standard deviations of 0.2–13.6%. The m-PFC method can greatly improve the efficiency of sample pretreatment. Furthermore, this work provides methodological guidance on how to select cleanup materials and allocate their proportions.

Preparative isolation of the major metabolite NK-1375 of diamide insecticide cyclaniliprole and its application to pertinent residue analysis in plant-origin foods using UHPLC-MS/MS.

NK-1375 is a major metabolite of the diamide insecticide cyclaniliprole (CYCP) with toxicological significance. It is formed in various transformation pathways of CYCP, including photolysis and plant metabolism. In the present study, NK-1375 was produced employing the liquid-phase photolysis of CYCP followed by isolation using preparative liquid chromatography. The structure of the isolated substance was confirmed using MS and 1 H NMR spectroscopy, and its purity was measured to be 95.9% using HPLC. As its application, a residue analysis method was first developed for the simultaneous determination of CYCP and NK-1375 in six representative plant-origin foods using fast multi-plug filtration cleanup and UHPLC-MS/MS. Excellent linearity (r > 0.999) was obtained over the calibration range from 0.001 to 0.1 μg mL-1 . The recoveries (intra-day and inter-day) of CYCP and NK-1375 from different matrices ranged from 74 to 112%, with corresponding relative standard deviations less than 13%. The limits of quantitation of these two compounds were defined at 0.01 mg kg-1 . This study can be useful for the subsequent analytical or toxicological research on this important pesticide metabolite.

Determination of 10 pyrethroid pesticide residues in tea by gas chromatography-tandem mass spectrometry coupled with multi-plug filtration cleanup

A method for the determination of 10 pyrethroid pesticide residues in tea was established by multi-plug filtration cleanup (m-PFC) method combined with gas chromatography-tandem mass spectrometry (GC-MS/MS). Different extraction solvents (acetonitrile, acetone and ethyl acetate) and extraction methods (immersion without water and immersion with water) were compared. The effect of two kinds of QuEChERS pipes and m-PFC column on the purification of tea extracts and the pesticide recoveries were compared. The results showed that the tea samples could be extracted most efficiently when using acetonitrile without immersion in water. The m-PFC column had a good purification effect on the tea extract and could guarantee a high recovery rate. Good linear relationships were observed for the 10 pyrethroid pesticides, and the correlation coefficients (R2) were greater than0.9980. The average recoveries for the 10 pyrethroid pesticides were in the range of 87.5%-111.3% at four spiked levels, and the RSDs were in the range of 2.1%-8.9%. The LODs and LOQs were 0.001-0.015 mg/kg and 0.003-0.05 mg/kg, respectively. The method was applied to the determination of the 10 pyrethroid pesticides in 50 tea samples. The detection rate of the pyrethroid pesticides was 48%, but all the pesticide residues were below the national standard limits. Compared with the traditional QuEChERS and solid phase extraction methods, this method has the advantages of operational simplicity as well as high accuracy and good precision. The establishment of this method provides a new strategy for the rapid detection of pyrethroid pesticide residues in tea.

Dual-layer column filtration cleanup and gas chromatography-tandem mass spectrometry detection for the analysis of 39 pesticide residues in porcine meat.

A rapid and effective method was developed for the analysis of 39 pesticide residues in porcine meat with dual-layer multiplug filtration cleanup and gas chromatography-tandem mass spectrometry detection. The cleanup process was performed with columns packed with two layers, namely multiwalled carbon nanotubes, C18 and anhydrous magnesium sulfate (MgSO4 ) as top layer, while mixture of florisil and MgSO4 as bottom layer. A single-layer method was tested in parallel, with columns packed with the same amount of absorbents. Extraction conditions and filtration cleanup process were optimized to obtain satisfied method performance. Method linearity was calculated with coefficients of determination more than 0.995. The limits of quantitation were verified with acceptable accuracy at the lowest spiked concentration of 0.01mg/kg (except pyrimethanil). The recoveries at three fortified levels (0.01, 0.05, and 0.1mg/kg) in five replicates were between 74 and 118% (except pyrimethanil) with relative standard deviations range from 1 to 16%. The matrix effects were in the range of 1.01 to 2.84. This new method was applied for the analysis of multipesticide residues in market samples of porcine meat. This study showed the dual-layer multiplug filtration cleanup demonstrated better performance than that with the single-layer columns in cleanup of porcine meat.

Development and evaluation of an automated multi-channel multiplug filtration cleanup device for pesticide residue analysis on mulberry leaves and processed tea.

An automated multi-channel multiplug filtration cleanup (m-PFC) device was designed and developed. m-PFC columns were suitably installed in the device. The cycle times, speed and nitrogen pressure parameters of the m-PFC column were optimized. The device was utilized to analyze the 82 pesticide residues in fresh mulberry leaves and processed tea with GC-MS/MS detection. Method validation was performed on 82 pesticide residues in fresh mulberry leaves and processed tea at spiked levels of 0.01, 0.05 and 0.5 mg kg−1. The fortified recoveries of 82 pesticides were 72–115% and the relative standard deviations were 1–15%, except for diniconazole and clodinafop-propargyl in mulberry leaves. The automated multi-channel m-PFC device was successfully applied to detect the pesticide residues in fresh mulberry leaves and processed tea samples. With comparison to the conventional QuEChERS method, the current method using this device did not need additional vortex or centrifugation steps, and could process 48–64 samples in about one hour. The automated m-PFC method saved labor and improved the precision and was shown to be efficient and practical in pesticide residue analysis.

Performance comparison of dispersive solid-phase extraction and multiplug filtration cleanup methods for the determination of tefuryltrione in plant and environmental samples using UHPLC-MS/MS.

The detection frequencies of tefuryltrione, a new type of 4-hydroxyphenyl-pyruvate dioxygenase inhibitor herbicide, are rarely reported, probably because of the paucity of analytical methods. Herein, an effective and sensitive analytical method has been developed to detect tefuryltrione in vegetables (tomato and cucumber), cereals (rice and corn), soil, and water by ultra high performance liquid chromatography coupled with tandem mass spectrometry. Comparisons of the performances of dispersive solid-phase extraction and multiplug filtration cleanup methods were carried out for tefuryltrione in complex matrices. Extraction solvents and purification sorbents were further optimized for dispersive solid-phase extraction. Tefuryltrione was analyzed with electrospray ionization in the positive mode within 2.0min. Mean recoveries for tefuryltrione were 75.4-108.9% with relative standard deviations less than 11.0% at three fortification levels (10, 100, 500μg/kg) in the sample matrixes. Limits of quantification ranged from 0.70 to 5.12μg/kg, and an excellent linearity (R2 ≥ 0.9902) was obtained for tefuryltrione at concentrations of 5-1000μg/L. The results showed that the developed dispersive solid-phase extraction method could serve as an effective, sensitive, and robust method for routine monitoring of tefuryltrione residue in plants and environmental samples.

Simultaneous determination of 124 pesticide residues in Chinese liquor and liquor-making raw materials (sorghum and rice hull) by rapid Multi-plug Filtration Cleanup and gas chromatography–tandem mass spectrometry

A multi-residue method was developed for the determination of 124 pesticide residues in Chinese liquor and liquor-making raw materials (sorghum and rice hull) by rapid Multi-plug Filtration Cleanup (m-PFC) and GC–MS/MS detection. Different combination and proportion sets of sorbents were initially optimized for each matrix with adispersive solid-phase extraction (d-SPE) procedure. Satisfactory linearity was obtained for the 124 pesticides with regression coefficients (R2) greater than 0.9901. Mean recoveries of 121 pesticides were in the range of 71–121% with Relative Standard Deviations (RSDs) lower than 16.8% except cyprodinil, diflufenican and prothioconazole. The Limit of Quantification (LOQs) was in the range of 1.0×10−4–5.0×10−3mgkg−1 and the Limit of Detection (LODs) ranged from 3.0×10−5 to 1.5×10−3mgkg−1 for the 124 pesticides in the matrices. It is demonstrated the m-PFC procedure is superior to the d-SPE method and it could be used to routinely monitor of pesticide residues in market samples.

Analysis of sulfonamides, tilmicosin and avermectins residues in typical animal matrices with multi-plug filtration cleanup by liquid chromatography-tandem mass spectrometry detection.

The frequent use of various veterinary drugs could lead to residue bioaccumulation in animal tissues, which could cause dietary risks to human health. In order to quickly analyze the residues, a liquid chromatography tandem mass spectrometry (LC-MS/MS) method was developed for detecting Sulfonamides, Tilmicosin and Avermectins (AVMs) residues in animal samples. For sample preparation, modified QuEChERS (quick, easy, cheap, effective, rugged and safe) and ultrasound-assisted extraction (UAE) methods were used. For sample cleanup, n-Hexane delipidation and multi-plug filtration cleanup (m-PFC) method based on primary-secondary amine (PSA) and octadecyl-silica (C18) were used, followed by LC-MS/MS analysis. It was validated on 7 animal matrices (bovine, caprine, swine meat and their kidneys, milk) at two fortified concentration levels of 5 and 100μg/kg. The recoveries ranged from 82 to 107% for all analytes with relative standard deviations (RSDs) less than 15%. Matrix-matched calibrations were performed with coefficients of determination above 0.998 for all analytes within concentration levels of 5-500μg/kg. The developed method was successfully used to analysis veterinary drugs of real animal samples from local markets.