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Comparison of the efficiency of different extraction methods for the simultaneous determination of mycotoxins and pesticides in milk samples by ultra high-performance liquid chromatography-tandem mass spectrometry
A rapid multi-analyte method has been developed for the simultaneous determination of pesticides and mycotoxins in milk by ultra high-performance liquid chromatography coupled to triple quadrupole mass spectrometry (UHPLC-QqQ-MS/MS). A variety of methodologies has been evaluated, including solid-pha...
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| Published in: | Analytical and bioanalytical chemistry 2011-03, Vol.399 (8), p.2863-2875 |
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| cited_by | cdi_FETCH-LOGICAL-c501t-914f867d9bc71fe69738389b3d06a27c138c90696e1f2c0013d61ca265968ace3 |
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| cites | cdi_FETCH-LOGICAL-c501t-914f867d9bc71fe69738389b3d06a27c138c90696e1f2c0013d61ca265968ace3 |
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| container_issue | 8 |
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| container_title | Analytical and bioanalytical chemistry |
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| creator | Aguilera-Luiz, M. M Plaza-Bolaños, P Romero-González, R Martínez Vidal, J. L Frenich, A. Garrido |
| description | A rapid multi-analyte method has been developed for the simultaneous determination of pesticides and mycotoxins in milk by ultra high-performance liquid chromatography coupled to triple quadrupole mass spectrometry (UHPLC-QqQ-MS/MS). A variety of methodologies has been evaluated, including solid-phase extraction (SPE), “dilute-and-shoot” (liquid-liquid extraction-based procedures), and QuEChERS (quick, easy, cheap, effective, rugged, and safe)-based methods. The optimization and development process was carried out considering that the maximum residue level for aflatoxin M1 (AFM1) in milk in the European Union (EU) is set at 0.05 μg kg⁻¹, which is the lowest tolerance in the target compounds. The selected method consisted of an extraction by SPE using C18 as sorbent and methanol as elution solvent. The final determination was performed by UHPLC-QqQ-MS/MS. Matrix-matched standard calibration was used for quantification, obtaining recoveries in the range 60-120% with relative standard deviations |
| doi_str_mv | 10.1007/s00216-011-4670-7 |
| format | article |
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M ; Plaza-Bolaños, P ; Romero-González, R ; Martínez Vidal, J. L ; Frenich, A. Garrido</creator><creatorcontrib>Aguilera-Luiz, M. M ; Plaza-Bolaños, P ; Romero-González, R ; Martínez Vidal, J. L ; Frenich, A. Garrido</creatorcontrib><description>A rapid multi-analyte method has been developed for the simultaneous determination of pesticides and mycotoxins in milk by ultra high-performance liquid chromatography coupled to triple quadrupole mass spectrometry (UHPLC-QqQ-MS/MS). A variety of methodologies has been evaluated, including solid-phase extraction (SPE), “dilute-and-shoot” (liquid-liquid extraction-based procedures), and QuEChERS (quick, easy, cheap, effective, rugged, and safe)-based methods. The optimization and development process was carried out considering that the maximum residue level for aflatoxin M1 (AFM1) in milk in the European Union (EU) is set at 0.05 μg kg⁻¹, which is the lowest tolerance in the target compounds. The selected method consisted of an extraction by SPE using C18 as sorbent and methanol as elution solvent. The final determination was performed by UHPLC-QqQ-MS/MS. Matrix-matched standard calibration was used for quantification, obtaining recoveries in the range 60-120% with relative standard deviations <25%, at three spiking levels: 0.5, 10, and 50 μg kg⁻¹ (ten times lower for AFM1). Limits of quantification ranged from 0.20 to 0.67 μg kg⁻¹, which were always below or equal to the established tolerance levels by the EU. 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M</creatorcontrib><creatorcontrib>Plaza-Bolaños, P</creatorcontrib><creatorcontrib>Romero-González, R</creatorcontrib><creatorcontrib>Martínez Vidal, J. L</creatorcontrib><creatorcontrib>Frenich, A. Garrido</creatorcontrib><title>Comparison of the efficiency of different extraction methods for the simultaneous determination of mycotoxins and pesticides in milk samples by ultra high-performance liquid chromatography-tandem mass spectrometry</title><title>Analytical and bioanalytical chemistry</title><addtitle>Anal Bioanal Chem</addtitle><addtitle>Anal Bioanal Chem</addtitle><description>A rapid multi-analyte method has been developed for the simultaneous determination of pesticides and mycotoxins in milk by ultra high-performance liquid chromatography coupled to triple quadrupole mass spectrometry (UHPLC-QqQ-MS/MS). 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Finally, the selected method was applied to different types of milk.</description><subject>Analysis</subject><subject>Analytical Chemistry</subject><subject>Animals</subject><subject>Biochemistry</subject><subject>Cattle</subject><subject>Characterization and Evaluation of Materials</subject><subject>Chemistry</subject><subject>Chemistry and Materials Science</subject><subject>Chromatographic methods and physical methods associated with chromatography</subject><subject>Chromatography, High Pressure Liquid - methods</subject><subject>Exact sciences and technology</subject><subject>Extraction</subject><subject>Food Contamination - analysis</subject><subject>Food Science</subject><subject>High performance liquid chromatography</subject><subject>Laboratory Medicine</subject><subject>Liquid chromatography</subject><subject>Mass spectrometry</subject><subject>Methods</subject><subject>Methyl alcohol</subject><subject>Milk</subject><subject>Milk - chemistry</subject><subject>Monitoring/Environmental Analysis</subject><subject>Mycotoxins</subject><subject>Mycotoxins - analysis</subject><subject>Original Paper</subject><subject>Other chromatographic methods</subject><subject>Pesticide Residues - analysis</subject><subject>Pesticides</subject><subject>SPE</subject><subject>Spectrometric and optical methods</subject><subject>Tandem Mass Spectrometry - methods</subject><subject>Tolerances</subject><subject>UHPLC-QqQ-MS/MS</subject><issn>1618-2642</issn><issn>1618-2650</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2011</creationdate><recordtype>article</recordtype><recordid>eNqFkstu1TAQhiMEoqXwAGzAGwSbFDsXx15WR9ykSiyga8vHGZ-4xHZqO1LzoLwPzsmh7Iq8iGN__8z4nymK1wRfEoy7jxHjitASE1I2tMNl96Q4J5SwsqItfvqwb6qz4kWMtxiTlhH6vDirSMUo5fi8-L3zdpLBRO-Q1ygNgEBroww4tawnvdEaAriE4D4FqZLJpIU0-D4i7cNREo2dxyQd-DmiHhIEa5w8ojmEXZRP_t64iKTr0QQx5QQ9RGRyKDP-QlHaacz_-wXlOEGiwRyGcoKQE1jpFKDR3M2mR2oI3srkD0FOw1LmlD1YZGWMKE6gUr6FFJaXxTMtxwivTt-L4ubzp5-7r-X19y_fdlfXpWoxSSUnjWa06_ledUQD5V3Nasb3dY-prDpFaqY4ppwC0ZXK9tU9JUpmdzllUkF9Ubzf4k7B3835XcKaqGAcNysEY5i2BNf8_2RbN12VO5nJD4-SpGuaDhPMV_RyQw9yBGGc9muH8sqmGOUdaJPPr2reNRVeX3dRkE2ggo8xgBZTMFaGRRAs1pES20iJXIhYR0qsmjeneua9hf5B8XeGMvDuBMio5KhDbpiJ_7iaY8aP1VYbF_OVO0AQt34OLvfn0exvN5GWXshDHlRx8yP7VGPCm7ZipP4DfYXx-A</recordid><startdate>20110301</startdate><enddate>20110301</enddate><creator>Aguilera-Luiz, M. 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M ; Plaza-Bolaños, P ; Romero-González, R ; Martínez Vidal, J. L ; Frenich, A. 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A variety of methodologies has been evaluated, including solid-phase extraction (SPE), “dilute-and-shoot” (liquid-liquid extraction-based procedures), and QuEChERS (quick, easy, cheap, effective, rugged, and safe)-based methods. The optimization and development process was carried out considering that the maximum residue level for aflatoxin M1 (AFM1) in milk in the European Union (EU) is set at 0.05 μg kg⁻¹, which is the lowest tolerance in the target compounds. The selected method consisted of an extraction by SPE using C18 as sorbent and methanol as elution solvent. The final determination was performed by UHPLC-QqQ-MS/MS. Matrix-matched standard calibration was used for quantification, obtaining recoveries in the range 60-120% with relative standard deviations <25%, at three spiking levels: 0.5, 10, and 50 μg kg⁻¹ (ten times lower for AFM1). Limits of quantification ranged from 0.20 to 0.67 μg kg⁻¹, which were always below or equal to the established tolerance levels by the EU. 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| subjects | Analysis Analytical Chemistry Animals Biochemistry Cattle Characterization and Evaluation of Materials Chemistry Chemistry and Materials Science Chromatographic methods and physical methods associated with chromatography Chromatography, High Pressure Liquid - methods Exact sciences and technology Extraction Food Contamination - analysis Food Science High performance liquid chromatography Laboratory Medicine Liquid chromatography Mass spectrometry Methods Methyl alcohol Milk Milk - chemistry Monitoring/Environmental Analysis Mycotoxins Mycotoxins - analysis Original Paper Other chromatographic methods Pesticide Residues - analysis Pesticides SPE Spectrometric and optical methods Tandem Mass Spectrometry - methods Tolerances UHPLC-QqQ-MS/MS |
| title | Comparison of the efficiency of different extraction methods for the simultaneous determination of mycotoxins and pesticides in milk samples by ultra high-performance liquid chromatography-tandem mass spectrometry |
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