Conclusions
A new rapid and sensitive LC–MS/MS method has been developed and validated for the simultaneous determination of the six most prominent ergot alkaloids, ergometrine, ergosine, ergotamine, ergocornine, ergokryptine and ergocristine, as well as their corresponding epimers in food and feed samples. The suitability of a mixture of ethyl acetate and methanol as extraction solvent under alkaline conditions, as well as the efficiency of liquid–liquid partitioning as sample clean-up approach were demonstrated. Methanol also proved to be a suitable alternative to acetonitrile for its use as organic modifier, as the former gave enhanced MS signal. The stability of an XBridge stationary phase allows the use of an alkaline mobile phase, thereby improving the chromatographic separation of the ergot alkaloids. The application of a simple sample clean-up protocol and a careful selection of the sample solvent allow minimising the epimerization of the ergot alkaloids during analysis. A major strength of the proposed method is the low limits of detection and of quantification, and its applicability to a wide range of food and feed matrices. In addition, the method also has the advantages of being rapid, simple and suitable for routinely determination of ergot alkaloids in various matrices. The levels of ergot alkaloids (1–1145 μg/kg for the total ergot alkaloid content) found in the samples from the Belgian food and feed supply are in some cases comparable to those reported in surveys from other countries, and confirm the need for a risk assessment for humans and animals. Besides the monitoring of ergot alkaloids in foods and feeds, the proposed method is being implemented to support the development of a molecularly imprinted polymer for ergot alkaloids (Lenain et al., 2010), and it also represents a suitable tool for further research and study of the ergot problem.
ConclusionsA new rapid and sensitive LC–MS/MS method has been developed and validated for the simultaneous determination of the six most prominent ergot alkaloids, ergometrine, ergosine, ergotamine, ergocornine, ergokryptine and ergocristine, as well as their corresponding epimers in food and feed samples. The suitability of a mixture of ethyl acetate and methanol as extraction solvent under alkaline conditions, as well as the efficiency of liquid–liquid partitioning as sample clean-up approach were demonstrated. Methanol also proved to be a suitable alternative to acetonitrile for its use as organic modifier, as the former gave enhanced MS signal. The stability of an XBridge stationary phase allows the use of an alkaline mobile phase, thereby improving the chromatographic separation of the ergot alkaloids. The application of a simple sample clean-up protocol and a careful selection of the sample solvent allow minimising the epimerization of the ergot alkaloids during analysis. A major strength of the proposed method is the low limits of detection and of quantification, and its applicability to a wide range of food and feed matrices. In addition, the method also has the advantages of being rapid, simple and suitable for routinely determination of ergot alkaloids in various matrices. The levels of ergot alkaloids (1–1145 μg/kg for the total ergot alkaloid content) found in the samples from the Belgian food and feed supply are in some cases comparable to those reported in surveys from other countries, and confirm the need for a risk assessment for humans and animals. Besides the monitoring of ergot alkaloids in foods and feeds, the proposed method is being implemented to support the development of a molecularly imprinted polymer for ergot alkaloids (Lenain et al., 2010), and it also represents a suitable tool for further research and study of the ergot problem.
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Conclusions
A New Rapid and sensitive LC-MS / MS method has been developed and Validated for the Simultaneous determination of the Six Most prominent ergot alkaloids, ergometrine, Ergosine, ergotamine, Ergocornine, Ergokryptine and Ergocristine, as well as their corresponding Epimers in Food and. feed samples. The suitability of a mixture of ethyl acetate and methanol as extraction solvent under alkaline conditions, as well as the efficiency of liquid-liquid partitioning as sample clean-up approach were demonstrated. Methanol also proved to be a suitable alternative to acetonitrile for its use as organic modifier, as the former gave enhanced MS signal. The stability of an XBridge stationary phase allows the use of an alkaline mobile phase, thereby improving the chromatographic separation of the ergot alkaloids. The application of a simple sample clean-up protocol and a careful selection of the sample solvent allow minimising the epimerization of the ergot alkaloids during analysis. A major strength of the proposed method is the low limits of detection and of quantification, and its applicability to a wide range of food and feed matrices. In addition, the method also has the advantages of being rapid, simple and suitable for routinely determination of ergot alkaloids in various matrices. The levels of ergot alkaloids (1-1145 μg / kg for the total ergot alkaloid content) found in the samples from the Belgian food and feed supply are in some cases comparable to those reported in surveys from other countries, and confirm the need for a. risk assessment for humans and animals. Besides the monitoring of ergot alkaloids in foods and feeds, the proposed method is being implemented to support the development of a molecularly imprinted polymer for ergot alkaloids (Lenain et al., 2010), and it also represents a suitable tool for further research and study. of the ergot problem.
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Conclusions
A new rapid and sensitive LC - MS / MS method has been developed and validated for the simultaneous determination. Of the six most prominent ergot alkaloids ergometrine ergosine ergotamine,,,,,, ergocornine ergokryptine and ergocristine. As well as their corresponding epimers in food and feed samples.The suitability of a mixture of ethyl acetate and methanol as extraction solvent under, alkaline conditions as well as. The efficiency of liquid - liquid partitioning as sample clean-up approach were demonstrated. Methanol also proved to be a. Suitable alternative to acetonitrile for its use as, organic modifier as the former gave enhanced MS signal.The stability of an XBridge stationary phase allows the use of an alkaline, mobile phase thereby improving the chromatographic. Separation of the ergot alkaloids. The application of a simple sample clean-up protocol and a careful selection of the sample. Solvent allow minimising the epimerization of the ergot alkaloids during analysis.A major strength of the proposed method is the low limits of detection and, of quantification and its applicability to. A wide range of food and feed matrices. In addition the method, also has the advantages of being rapid simple and, suitable. For routinely determination of ergot alkaloids in various matrices.The levels of ergot alkaloids (1 - 1145 thermal g / kg for the total ergot alkaloid content) found in the samples from the Belgian. Food and feed supply are in some cases comparable to those reported in surveys from, other countries and confirm the need. For a risk assessment for humans and animals. Besides the monitoring of ergot alkaloids in foods, and feedsThe proposed method is being implemented to support the development of a molecularly imprinted polymer for ergot alkaloids. (Lenain et al, 2010), and it also represents a suitable tool for further research and study of the ergot problem.
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