Development of a new LC-MS method for accurate and sensitive determination of 33 pyrrolizidine and 21 tropane alkaloids in plant-based food matrices
Setting of maximum limits for a number of plant alkaloids is under discussion in the EU. The novel method developed and optimized in this study enables simultaneous determination of 21 tropane alkaloids (TAs) and 33 pyrrolizidine (PAs) together with their N-oxides (PANOs). For analysis of aqueous-me...
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| Veröffentlicht in: | Analytical and bioanalytical chemistry 2020-10, Vol.412 (26), p.7155-7167 |
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| creator | Dzuman, Zbynek Jonatova, Petra Stranska-Zachariasova, Milena Prusova, Nela Brabenec, Ondrej Novakova, Alena Fenclova, Marie Hajslova, Jana |
| description | Setting of maximum limits for a number of plant alkaloids is under discussion in the EU. The novel method developed and optimized in this study enables simultaneous determination of 21 tropane alkaloids (TAs) and 33 pyrrolizidine (PAs) together with their N-oxides (PANOs). For analysis of aqueous-methanolic extract, reversed phase ultra-high-performance liquid chromatography and tandem mass spectrometry (RP-U-HPLC-MS/MS) was employed. The method was validated for frequently contaminated matrices (i) sorghum, (ii) oregano, and (iii) mixed herbal tea. The recoveries at two spiking levels were in the range of 82–115%, 80–106%, and 78–117%, respectively, and repeatabilities were less than 19% for all analyte/matrix combinations. As regards the achieved limits of quantification (LOQ), their values were in the range of 0.5–10 μg kg
−1
. The crucial problem encountered during method development, co-elution of multiple groups of isomeric alkaloids, was overcome by subsequent sample separation in the second chromatographic system, hydrophilic interaction liquid chromatography (HILIC), providing different separation selectivity. Lycopsamine, echinatine, and indicine (co-elution group 1) and N-oxides of indicine and intermedine (co-elution group 2), which could not be resolved on the commonly used RP column, were possible to separate fully by using the HILIC system. |
| doi_str_mv | 10.1007/s00216-020-02848-6 |
| format | Article |
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−1
. The crucial problem encountered during method development, co-elution of multiple groups of isomeric alkaloids, was overcome by subsequent sample separation in the second chromatographic system, hydrophilic interaction liquid chromatography (HILIC), providing different separation selectivity. Lycopsamine, echinatine, and indicine (co-elution group 1) and N-oxides of indicine and intermedine (co-elution group 2), which could not be resolved on the commonly used RP column, were possible to separate fully by using the HILIC system.</description><identifier>ISSN: 1618-2642</identifier><identifier>EISSN: 1618-2650</identifier><identifier>DOI: 10.1007/s00216-020-02848-6</identifier><identifier>PMID: 32803302</identifier><language>eng</language><publisher>Berlin/Heidelberg: Springer Berlin Heidelberg</publisher><subject>Alkaloids ; Alkaloids - analysis ; Analysis ; Analytical Chemistry ; Biochemistry ; Characterization and Evaluation of Materials ; Chemistry ; Chemistry and Materials Science ; Chromatography ; Chromatography, High Pressure Liquid - methods ; Elution ; Food Contamination - analysis ; Food plants ; Food Science ; Herbal tea ; High performance liquid chromatography ; Ions ; Isomerism ; Laboratory Medicine ; Limit of Detection ; Liquid chromatography ; Mass spectrometry ; Mass spectroscopy ; Methods ; Monitoring/Environmental Analysis ; N-Oxides ; Oregano ; Oxides ; Plant-based foods ; Plants - chemistry ; Pyrrolizidine alkaloids ; Pyrrolizidine Alkaloids - analysis ; Reproducibility of Results ; Research Paper ; Selectivity ; Separation ; Sorghum ; Tandem Mass Spectrometry - methods ; Tea ; Tropane alkaloids ; Tropanes - analysis</subject><ispartof>Analytical and bioanalytical chemistry, 2020-10, Vol.412 (26), p.7155-7167</ispartof><rights>Springer-Verlag GmbH Germany, part of Springer Nature 2020</rights><rights>COPYRIGHT 2020 Springer</rights><rights>Springer-Verlag GmbH Germany, part of Springer Nature 2020.</rights><lds50>peer_reviewed</lds50><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c451t-60b3a274df533291a68dcdd6239ff9b80cb30b4a610bcabb76a77a3e0d34449b3</citedby><cites>FETCH-LOGICAL-c451t-60b3a274df533291a68dcdd6239ff9b80cb30b4a610bcabb76a77a3e0d34449b3</cites></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><linktopdf>$$Uhttps://link.springer.com/content/pdf/10.1007/s00216-020-02848-6$$EPDF$$P50$$Gspringer$$H</linktopdf><linktohtml>$$Uhttps://link.springer.com/10.1007/s00216-020-02848-6$$EHTML$$P50$$Gspringer$$H</linktohtml><link.rule.ids>314,780,784,27924,27925,41488,42557,51319</link.rule.ids><backlink>$$Uhttps://www.ncbi.nlm.nih.gov/pubmed/32803302$$D View this record in MEDLINE/PubMed$$Hfree_for_read</backlink></links><search><creatorcontrib>Dzuman, Zbynek</creatorcontrib><creatorcontrib>Jonatova, Petra</creatorcontrib><creatorcontrib>Stranska-Zachariasova, Milena</creatorcontrib><creatorcontrib>Prusova, Nela</creatorcontrib><creatorcontrib>Brabenec, Ondrej</creatorcontrib><creatorcontrib>Novakova, Alena</creatorcontrib><creatorcontrib>Fenclova, Marie</creatorcontrib><creatorcontrib>Hajslova, Jana</creatorcontrib><title>Development of a new LC-MS method for accurate and sensitive determination of 33 pyrrolizidine and 21 tropane alkaloids in plant-based food matrices</title><title>Analytical and bioanalytical chemistry</title><addtitle>Anal Bioanal Chem</addtitle><addtitle>Anal Bioanal Chem</addtitle><description>Setting of maximum limits for a number of plant alkaloids is under discussion in the EU. The novel method developed and optimized in this study enables simultaneous determination of 21 tropane alkaloids (TAs) and 33 pyrrolizidine (PAs) together with their N-oxides (PANOs). For analysis of aqueous-methanolic extract, reversed phase ultra-high-performance liquid chromatography and tandem mass spectrometry (RP-U-HPLC-MS/MS) was employed. The method was validated for frequently contaminated matrices (i) sorghum, (ii) oregano, and (iii) mixed herbal tea. The recoveries at two spiking levels were in the range of 82–115%, 80–106%, and 78–117%, respectively, and repeatabilities were less than 19% for all analyte/matrix combinations. As regards the achieved limits of quantification (LOQ), their values were in the range of 0.5–10 μg kg
−1
. The crucial problem encountered during method development, co-elution of multiple groups of isomeric alkaloids, was overcome by subsequent sample separation in the second chromatographic system, hydrophilic interaction liquid chromatography (HILIC), providing different separation selectivity. Lycopsamine, echinatine, and indicine (co-elution group 1) and N-oxides of indicine and intermedine (co-elution group 2), which could not be resolved on the commonly used RP column, were possible to separate fully by using the HILIC system.</description><subject>Alkaloids</subject><subject>Alkaloids - analysis</subject><subject>Analysis</subject><subject>Analytical Chemistry</subject><subject>Biochemistry</subject><subject>Characterization and Evaluation of Materials</subject><subject>Chemistry</subject><subject>Chemistry and Materials Science</subject><subject>Chromatography</subject><subject>Chromatography, High Pressure Liquid - methods</subject><subject>Elution</subject><subject>Food Contamination - analysis</subject><subject>Food plants</subject><subject>Food Science</subject><subject>Herbal tea</subject><subject>High performance liquid chromatography</subject><subject>Ions</subject><subject>Isomerism</subject><subject>Laboratory Medicine</subject><subject>Limit of Detection</subject><subject>Liquid chromatography</subject><subject>Mass spectrometry</subject><subject>Mass spectroscopy</subject><subject>Methods</subject><subject>Monitoring/Environmental Analysis</subject><subject>N-Oxides</subject><subject>Oregano</subject><subject>Oxides</subject><subject>Plant-based foods</subject><subject>Plants - 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Academic</collection><jtitle>Analytical and bioanalytical chemistry</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Dzuman, Zbynek</au><au>Jonatova, Petra</au><au>Stranska-Zachariasova, Milena</au><au>Prusova, Nela</au><au>Brabenec, Ondrej</au><au>Novakova, Alena</au><au>Fenclova, Marie</au><au>Hajslova, Jana</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Development of a new LC-MS method for accurate and sensitive determination of 33 pyrrolizidine and 21 tropane alkaloids in plant-based food matrices</atitle><jtitle>Analytical and bioanalytical chemistry</jtitle><stitle>Anal Bioanal Chem</stitle><addtitle>Anal Bioanal Chem</addtitle><date>2020-10-01</date><risdate>2020</risdate><volume>412</volume><issue>26</issue><spage>7155</spage><epage>7167</epage><pages>7155-7167</pages><issn>1618-2642</issn><eissn>1618-2650</eissn><abstract>Setting of maximum limits for a number of plant alkaloids is under discussion in the EU. The novel method developed and optimized in this study enables simultaneous determination of 21 tropane alkaloids (TAs) and 33 pyrrolizidine (PAs) together with their N-oxides (PANOs). For analysis of aqueous-methanolic extract, reversed phase ultra-high-performance liquid chromatography and tandem mass spectrometry (RP-U-HPLC-MS/MS) was employed. The method was validated for frequently contaminated matrices (i) sorghum, (ii) oregano, and (iii) mixed herbal tea. The recoveries at two spiking levels were in the range of 82–115%, 80–106%, and 78–117%, respectively, and repeatabilities were less than 19% for all analyte/matrix combinations. As regards the achieved limits of quantification (LOQ), their values were in the range of 0.5–10 μg kg
−1
. The crucial problem encountered during method development, co-elution of multiple groups of isomeric alkaloids, was overcome by subsequent sample separation in the second chromatographic system, hydrophilic interaction liquid chromatography (HILIC), providing different separation selectivity. Lycopsamine, echinatine, and indicine (co-elution group 1) and N-oxides of indicine and intermedine (co-elution group 2), which could not be resolved on the commonly used RP column, were possible to separate fully by using the HILIC system.</abstract><cop>Berlin/Heidelberg</cop><pub>Springer Berlin Heidelberg</pub><pmid>32803302</pmid><doi>10.1007/s00216-020-02848-6</doi><tpages>13</tpages></addata></record> |
| fulltext | fulltext |
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| issn | 1618-2642 1618-2650 |
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| source | MEDLINE; SpringerNature Journals |
| subjects | Alkaloids Alkaloids - analysis Analysis Analytical Chemistry Biochemistry Characterization and Evaluation of Materials Chemistry Chemistry and Materials Science Chromatography Chromatography, High Pressure Liquid - methods Elution Food Contamination - analysis Food plants Food Science Herbal tea High performance liquid chromatography Ions Isomerism Laboratory Medicine Limit of Detection Liquid chromatography Mass spectrometry Mass spectroscopy Methods Monitoring/Environmental Analysis N-Oxides Oregano Oxides Plant-based foods Plants - chemistry Pyrrolizidine alkaloids Pyrrolizidine Alkaloids - analysis Reproducibility of Results Research Paper Selectivity Separation Sorghum Tandem Mass Spectrometry - methods Tea Tropane alkaloids Tropanes - analysis |
| title | Development of a new LC-MS method for accurate and sensitive determination of 33 pyrrolizidine and 21 tropane alkaloids in plant-based food matrices |
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