Determination of Grayanotoxins in Biological Samples by LC-MS/MS

详细信息    查看全文

• 作者：Dirk M. Holstege ; Birgit Puschner ; and Tuong Le
• 刊名：Journal of Agricultural and Food Chemistry
• 出版年：2001
• 出版时间：March 2001
• 年：2001
• 卷：49
• 期：3
• 页码：1648 - 1651
• 全文大小：65K
• 年卷期：v.49,no.3(March 2001)
• ISSN：1520-5118

文摘

A rapid LC-MS/MS method was developed for the quantitative determination of grayanotoxins I,II, and III in rumen contents, feces, and urine. The grayanotoxins were extracted from solid sampleswith methanol. The methanol extract was diluted with water and cleaned up using a reversed phasesolid phase extraction column. HPLC separation was performed by reversed phase HPLC using agradient of water and methanol containing 1% acetic acid. Determination was by positive ionelectrospray ionization and ion trap tandem mass spectrometry. Grayanotoxin I quantitation wasbased on fragmentation of the sodium adduct ion at m/z 435 to a product ion at m/z 375.Grayanotoxins II and III were quantitated on the basis of fragmentation of the ion at m/z 335 tothe product ion at m/z 299. The method detection limits were 0.2 mages/entities/mgr.gif">g/g in rumen contents and fecesand 0.05 mages/entities/mgr.gif">g/g in urine. Fortifications at the detection limits and 10 times the detection limits ofbovine rumen contents, caprine feces, and ovine urine were recovered in the range 80-114%. Thediagnostic utility of the method was tested by analyzing samples submitted to the veterinarytoxicology laboratory.Keywords: Grayanotoxin; HPLC; mass spectrometry; LC-MS