Pyrrolizidine alkaloids in the food chain: development, validation, and application of a new HPLC-ESI-MS/MS sum parameter method.
Contamination of food and feed with pyrrolizidine alkaloids is currently discussed as a potential health risk. Here, we report the development of a new HPLC-ESI-MS/MS sum parameter method to quantitate the pyrrolizidine alkaloid content in complex food matrices. The procedure was validated for honey and culinary herbs. Isotopically labeled 7-O-9-O-dibutyroyl-[9,9-(2)H2]-retronecine was synthesized and utilized as an internal standard for validation and quantitation. The total pyrrolizidine alkaloid content of a sample is expressed as a single sum parameter: retronecine equivalents (RE). Ld/Lq for honey was 0.1 μg RE/kg/0.3 μg RE/kg. For culinary herbs, 1.0 μg RE/kg/3.0 μg RE/kg (dry weight, dw) and 0.1 μg RE/kg/0.3 μg RE/kg (fresh weight, fw) were determined, respectively. The new method was applied to analyze 21 herbal convenience products. Fifteen products (71%) were pyrrolizidine alkaloid positive showing pyrrolizidine alkaloid concentrations ranging from 0.9 to 74 μg RE/kg fw.
Institute of Pharmaceutical Biology, Technische Universität Braunschweig , Mendelssohnstr. 1, 38106 Braunschweig, Germany.
Luise
L
Cramer
Hans-Martin
HM
Schiebel
Ludger
L
Ernst
Till
T
Beuerle
D029683:Borago / Q000737:chemistry; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D005504:Food Analysis / Q000379:methods*; D005506:Food Contamination / Q000032:analysis*; D006722:Honey; D057230:Limit of Detection; D011763:Pyrrolizidine Alkaloids / Q000032:analysis* / Q000737:chemistry; D015203:Reproducibility of Results; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000379:methods*
C000590720:7-O-9-O-dibutyroyl-(9,9-2H2)-retronecine; D011763:Pyrrolizidine Alkaloids; C014795:retronecine