Multi-dye residue analysis of triarylmethane, xanthene, phenothiazine and phenoxazine dyes in fish tissues by ultra-performance liquid chromatography–tandem mass spectrometry
•A new UPLC–MS/MS method was developed for the quantification of illegal dyes in fish tissues.•Due to the presence of strong positively charged sulphur groups, attention was paid to the solid phase elution step.•The validation was performed according to standards of European Union (Directive 2002/65...
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| Veröffentlicht in: | Journal of chromatography. B, Analytical technologies in the biomedical and life sciences Jg. 953-954; S. 92 - 101 |
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| Format: | Journal Article |
| Sprache: | Englisch |
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Elsevier B.V
15.03.2014
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| ISSN: | 1570-0232, 1873-376X, 1873-376X |
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| Abstract | •A new UPLC–MS/MS method was developed for the quantification of illegal dyes in fish tissues.•Due to the presence of strong positively charged sulphur groups, attention was paid to the solid phase elution step.•The validation was performed according to standards of European Union (Directive 2002/657/EC) and scientific literature.•The method was able to quantify at 0.25ngg−1.•Applicability of the method was shown in a subsequent monitoring study of wildlife eel in Flemish rivers.
Beside the possible illegal use of malachite green in aquaculture, other familiar dyes could also been applied by fraudulent producers due to their antiseptic and antibacterial activity. In this contribution, a new sensitive multi-residue method was developed to determine triarylmethane, xanthene, phenothiazine and phenoxazine dyes in fish by ultra-performance liquid chromatography–tandem mass spectrometry. Samples were extracted with acetonitrile, followed by an oxidation step using 2,3-dichloro-5,6-dicyanobenzoquinone. Further clean-up was performed by tandem solid phase extraction using weak and strong cation exchange cartridges. Extracts were analysed by UPLC-MSn operating in the positive electrospray ionisation mode (ESI+). The fourteen dyes were separated within only 12min on a C18 BEH column using 1mM ammonium acetate in water at pH 4.5 and acetonitrile as mobile phases at a flowrate of 0.4mLmin−1. The presented method was validated as defined by the European Union and scientific literature. Good linearity (R ≥0.99 and goodness-of-fit (g) ≤10%) was achieved over the tested concentration range (0.25–2ngg−1). Limit of quantification was 0.25ngg−1 for all dyes, with a signal-to-noise ratio of at least 10/1. This is at least 5 to 10 times lower than previous published methods. Limits of detection were all <0.1ngg−1. Precision and trueness fell within the criteria requested by the EC requirements for this concentration range. Decision limit (CCα) and detection capability (CCβ) were all <1 and <0.25ngg−1, respectively. Due to background levels of the xanthene dyes, the two rhodamine dyes could only be determined above 0.75ngg−1. For these dyes, the method can only be used for screening purposes. To show the applicability of the method, a monitoring study was performed to investigate the occurrence of artificial dyes in wildlife European eel in Flemish rivers |
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| AbstractList | Beside the possible illegal use of malachite green in aquaculture, other familiar dyes could also been applied by fraudulent producers due to their antiseptic and antibacterial activity. In this contribution, a new sensitive multi-residue method was developed to determine triarylmethane, xanthene, phenothiazine and phenoxazine dyes in fish by ultra-performance liquid chromatography-tandem mass spectrometry. Samples were extracted with acetonitrile, followed by an oxidation step using 2,3-dichloro-5,6-dicyanobenzoquinone. Further clean-up was performed by tandem solid phase extraction using weak and strong cation exchange cartridges. Extracts were analysed by UPLC-MSn operating in the positive electrospray ionisation mode (ESI+). The fourteen dyes were separated within only 12 min on a C18 BEH column using 1 mM ammonium acetate in water at pH 4.5 and acetonitrile as mobile phases at a flowrate of 0.4 mL min-1. The presented method was validated as defined by the European Union and scientific literature. Good linearity (R greater than or equal to 0.99 and goodness-of-fit (g) less than or equal to 10%) was achieved over the tested concentration range (0.25-2 ng g-1). Limit of quantification was 0.25 ng g-1 for all dyes, with a signal-to-noise ratio of at least 10/1. This is at least 5 to 10 times lower than previous published methods. Limits of detection were all <0.1 ng g-1. Precision and trueness fell within the criteria requested by the EC requirements for this concentration range. Decision limit (CC alpha ) and detection capability (CC beta ) were all <1 and <0.25 ng g-1, respectively. Due to background levels of the xanthene dyes, the two rhodamine dyes could only be determined above 0.75 ng g-1. For these dyes, the method can only be used for screening purposes. To show the applicability of the method, a monitoring study was performed to investigate the occurrence of artificial dyes in wildlife European eel in Flemish rivers •A new UPLC–MS/MS method was developed for the quantification of illegal dyes in fish tissues.•Due to the presence of strong positively charged sulphur groups, attention was paid to the solid phase elution step.•The validation was performed according to standards of European Union (Directive 2002/657/EC) and scientific literature.•The method was able to quantify at 0.25ngg−1.•Applicability of the method was shown in a subsequent monitoring study of wildlife eel in Flemish rivers. Beside the possible illegal use of malachite green in aquaculture, other familiar dyes could also been applied by fraudulent producers due to their antiseptic and antibacterial activity. In this contribution, a new sensitive multi-residue method was developed to determine triarylmethane, xanthene, phenothiazine and phenoxazine dyes in fish by ultra-performance liquid chromatography–tandem mass spectrometry. Samples were extracted with acetonitrile, followed by an oxidation step using 2,3-dichloro-5,6-dicyanobenzoquinone. Further clean-up was performed by tandem solid phase extraction using weak and strong cation exchange cartridges. Extracts were analysed by UPLC-MSn operating in the positive electrospray ionisation mode (ESI+). The fourteen dyes were separated within only 12min on a C18 BEH column using 1mM ammonium acetate in water at pH 4.5 and acetonitrile as mobile phases at a flowrate of 0.4mLmin−1. The presented method was validated as defined by the European Union and scientific literature. Good linearity (R ≥0.99 and goodness-of-fit (g) ≤10%) was achieved over the tested concentration range (0.25–2ngg−1). Limit of quantification was 0.25ngg−1 for all dyes, with a signal-to-noise ratio of at least 10/1. This is at least 5 to 10 times lower than previous published methods. Limits of detection were all <0.1ngg−1. Precision and trueness fell within the criteria requested by the EC requirements for this concentration range. Decision limit (CCα) and detection capability (CCβ) were all <1 and <0.25ngg−1, respectively. Due to background levels of the xanthene dyes, the two rhodamine dyes could only be determined above 0.75ngg−1. For these dyes, the method can only be used for screening purposes. To show the applicability of the method, a monitoring study was performed to investigate the occurrence of artificial dyes in wildlife European eel in Flemish rivers Beside the possible illegal use of malachite green in aquaculture, other familiar dyes could also been applied by fraudulent producers due to their antiseptic and antibacterial activity. In this contribution, a new sensitive multi-residue method was developed to determine triarylmethane, xanthene, phenothiazine and phenoxazine dyes in fish by ultra-performance liquid chromatography–tandem mass spectrometry. Samples were extracted with acetonitrile, followed by an oxidation step using 2,3-dichloro-5,6-dicyanobenzoquinone. Further clean-up was performed by tandem solid phase extraction using weak and strong cation exchange cartridges. Extracts were analysed by UPLC-MSn operating in the positive electrospray ionisation mode (ESI+). The fourteen dyes were separated within only 12min on a C18 BEH column using 1mM ammonium acetate in water at pH 4.5 and acetonitrile as mobile phases at a flowrate of 0.4mLmin−1. The presented method was validated as defined by the European Union and scientific literature. Good linearity (R ≥0.99 and goodness-of-fit (g) ≤10%) was achieved over the tested concentration range (0.25–2ngg−1). Limit of quantification was 0.25ngg−1 for all dyes, with a signal-to-noise ratio of at least 10/1. This is at least 5 to 10 times lower than previous published methods. Limits of detection were all <0.1ngg−1. Precision and trueness fell within the criteria requested by the EC requirements for this concentration range. Decision limit (CCα) and detection capability (CCβ) were all <1 and <0.25ngg−1, respectively. Due to background levels of the xanthene dyes, the two rhodamine dyes could only be determined above 0.75ngg−1. For these dyes, the method can only be used for screening purposes. To show the applicability of the method, a monitoring study was performed to investigate the occurrence of artificial dyes in wildlife European eel in Flemish rivers Beside the possible illegal use of malachite green in aquaculture, other familiar dyes could also been applied by fraudulent producers due to their antiseptic and antibacterial activity. In this contribution, a new sensitive multi-residue method was developed to determine triarylmethane, xanthene, phenothiazine and phenoxazine dyes in fish by ultra-performance liquid chromatography-tandem mass spectrometry. Samples were extracted with acetonitrile, followed by an oxidation step using 2,3-dichloro-5,6-dicyanobenzoquinone. Further clean-up was performed by tandem solid phase extraction using weak and strong cation exchange cartridges. Extracts were analysed by UPLC-MS(n) operating in the positive electrospray ionisation mode (ESI+). The fourteen dyes were separated within only 12min on a C18 BEH column using 1mM ammonium acetate in water at pH 4.5 and acetonitrile as mobile phases at a flowrate of 0.4mLmin(-1). The presented method was validated as defined by the European Union and scientific literature. Good linearity (R ≥0.99 and goodness-of-fit (g) ≤10%) was achieved over the tested concentration range (0.25-2ngg(-1)). Limit of quantification was 0.25ngg(-1) for all dyes, with a signal-to-noise ratio of at least 10/1. This is at least 5 to 10 times lower than previous published methods. Limits of detection were all <0.1ngg(-1). Precision and trueness fell within the criteria requested by the EC requirements for this concentration range. Decision limit (CCα) and detection capability (CCβ) were all <1 and <0.25ngg(-1), respectively. Due to background levels of the xanthene dyes, the two rhodamine dyes could only be determined above 0.75ngg(-1). For these dyes, the method can only be used for screening purposes. To show the applicability of the method, a monitoring study was performed to investigate the occurrence of artificial dyes in wildlife European eel in Flemish rivers. Beside the possible illegal use of malachite green in aquaculture, other familiar dyes could also been applied by fraudulent producers due to their antiseptic and antibacterial activity. In this contribution, a new sensitive multi-residue method was developed to determine triarylmethane, xanthene, phenothiazine and phenoxazine dyes in fish by ultra-performance liquid chromatography-tandem mass spectrometry. Samples were extracted with acetonitrile, followed by an oxidation step using 2,3-dichloro-5,6-dicyanobenzoquinone. Further clean-up was performed by tandem solid phase extraction using weak and strong cation exchange cartridges. Extracts were analysed by UPLC-MS(n) operating in the positive electrospray ionisation mode (ESI+). The fourteen dyes were separated within only 12min on a C18 BEH column using 1mM ammonium acetate in water at pH 4.5 and acetonitrile as mobile phases at a flowrate of 0.4mLmin(-1). The presented method was validated as defined by the European Union and scientific literature. Good linearity (R ≥0.99 and goodness-of-fit (g) ≤10%) was achieved over the tested concentration range (0.25-2ngg(-1)). Limit of quantification was 0.25ngg(-1) for all dyes, with a signal-to-noise ratio of at least 10/1. This is at least 5 to 10 times lower than previous published methods. Limits of detection were all <0.1ngg(-1). Precision and trueness fell within the criteria requested by the EC requirements for this concentration range. Decision limit (CCα) and detection capability (CCβ) were all <1 and <0.25ngg(-1), respectively. Due to background levels of the xanthene dyes, the two rhodamine dyes could only be determined above 0.75ngg(-1). For these dyes, the method can only be used for screening purposes. To show the applicability of the method, a monitoring study was performed to investigate the occurrence of artificial dyes in wildlife European eel in Flemish rivers.Beside the possible illegal use of malachite green in aquaculture, other familiar dyes could also been applied by fraudulent producers due to their antiseptic and antibacterial activity. In this contribution, a new sensitive multi-residue method was developed to determine triarylmethane, xanthene, phenothiazine and phenoxazine dyes in fish by ultra-performance liquid chromatography-tandem mass spectrometry. Samples were extracted with acetonitrile, followed by an oxidation step using 2,3-dichloro-5,6-dicyanobenzoquinone. Further clean-up was performed by tandem solid phase extraction using weak and strong cation exchange cartridges. Extracts were analysed by UPLC-MS(n) operating in the positive electrospray ionisation mode (ESI+). The fourteen dyes were separated within only 12min on a C18 BEH column using 1mM ammonium acetate in water at pH 4.5 and acetonitrile as mobile phases at a flowrate of 0.4mLmin(-1). The presented method was validated as defined by the European Union and scientific literature. Good linearity (R ≥0.99 and goodness-of-fit (g) ≤10%) was achieved over the tested concentration range (0.25-2ngg(-1)). Limit of quantification was 0.25ngg(-1) for all dyes, with a signal-to-noise ratio of at least 10/1. This is at least 5 to 10 times lower than previous published methods. Limits of detection were all <0.1ngg(-1). Precision and trueness fell within the criteria requested by the EC requirements for this concentration range. Decision limit (CCα) and detection capability (CCβ) were all <1 and <0.25ngg(-1), respectively. Due to background levels of the xanthene dyes, the two rhodamine dyes could only be determined above 0.75ngg(-1). For these dyes, the method can only be used for screening purposes. To show the applicability of the method, a monitoring study was performed to investigate the occurrence of artificial dyes in wildlife European eel in Flemish rivers. |
| Author | Reyns, Tim Belpaire, Claude Van Loco, Joris Geeraerts, Caroline |
| Author_xml | – sequence: 1 givenname: Tim surname: Reyns fullname: Reyns, Tim email: Tim.Reyns@wiv-isp.be organization: Scientific Institute of Public Health, Food, Medicines and Consumer Safety, Chemical Residues and Contaminants, Juliette Wytsmanstraat 14, 1050 Brussel, Belgium – sequence: 2 givenname: Claude surname: Belpaire fullname: Belpaire, Claude organization: Research Institute for Nature and Forest, Duboislaan 14, 1560 Groenendaal-Hoeilaart, Belgium – sequence: 3 givenname: Caroline surname: Geeraerts fullname: Geeraerts, Caroline organization: Research Institute for Nature and Forest, Gaverstraat 4, 9500 Geraardsbergen, Belgium – sequence: 4 givenname: Joris surname: Van Loco fullname: Van Loco, Joris organization: Scientific Institute of Public Health, Food, Medicines and Consumer Safety, Chemical Residues and Contaminants, Juliette Wytsmanstraat 14, 1050 Brussel, Belgium |
| BackLink | https://www.ncbi.nlm.nih.gov/pubmed/24583201$$D View this record in MEDLINE/PubMed |
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| Keywords | Crystal violet Residue analysis Dyes Ultra performance liquid chromatography–tandem mass spectrometry Aquaculture products Malachite green |
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| SSID | ssj0017073 |
| Score | 2.2318337 |
| Snippet | •A new UPLC–MS/MS method was developed for the quantification of illegal dyes in fish tissues.•Due to the presence of strong positively charged sulphur groups,... Beside the possible illegal use of malachite green in aquaculture, other familiar dyes could also been applied by fraudulent producers due to their antiseptic... |
| SourceID | proquest pubmed crossref elsevier |
| SourceType | Aggregation Database Index Database Enrichment Source Publisher |
| StartPage | 92 |
| SubjectTerms | Acetonitrile ammonium acetate Anguilla anguilla Animals antibacterial properties antiseptics Aquaculture Aquaculture products cation exchange Chromatography Chromatography, High Pressure Liquid - methods Coloring Agents - analysis Crystal violet detection limit Drug Residues - analysis Dyes Eels Fish Fishes ionization Linearity liquid chromatography Liquids Malachite green Mass spectrometry monitoring multiresidue analysis Muscles - chemistry Organic Chemicals - analysis oxidation phenothiazine Phenothiazines Regression Analysis Reproducibility of Results Residue analysis rivers screening Sensitivity and Specificity solid phase extraction tandem mass spectrometry Tandem Mass Spectrometry - methods Ultra performance liquid chromatography–tandem mass spectrometry wildlife |
| Title | Multi-dye residue analysis of triarylmethane, xanthene, phenothiazine and phenoxazine dyes in fish tissues by ultra-performance liquid chromatography–tandem mass spectrometry |
| URI | https://dx.doi.org/10.1016/j.jchromb.2014.02.002 https://www.ncbi.nlm.nih.gov/pubmed/24583201 https://www.proquest.com/docview/1508419932 https://www.proquest.com/docview/1531005923 https://www.proquest.com/docview/2000272262 |
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