title: UPLC TOF MS for sensitive quantification of naturally occurring pyrrolizidine alkaloids in Petasites hybridus extract (Ze 339).
abstract: Due to increasing regulatory awareness of their hepatotoxic, genotoxic and possibly carcinogenic potential, pyrrolizidine alkaloid (PA) content has to be thoroughly monitored in herbal medicinal preparations. Recently, new very low PA regulatory threshold concentrations have been requested by the authorities. Therefore, a highly sensitive and reproducible UPLC TOF MS method for the quantification of the PAs senkirkine, senecionine, seneciphylline, senecionine-N-oxide and seneciphylline-N-oxide in a CO2-extract of Petasites hybridus leaves (Ze 339) has been developed. The limit of quantification (LOQ) was 2ppb for all PAs. Recovery at the LOQ was between 88.9 and 141.9%, the repeatability precision between 3.5 and 13.6%. Linearity of the five PAs showed correlation coefficients between 0.9995 and 0.9998 and coefficients of variation between 7.44 and 8.56%. A working range between 2 ppb and 200 ppb could be fixed. In the tested batches of the P. hybridus extract Ze 339, the absence of PAs could be demonstrated. In conclusion, this assay allows to determine trace PA concentrations in P. hybridus extract Ze 339, making it suitable for analytical PA monitoring in accordance with regulatory requirements.
authors.affiliation: Departments of Analytical Development, Max Zeller Söhne AG, Seeblickstrasse 4, CH 8590 Romanshorn, Switzerland. Electronic address: alexander.schenk@zellerag.ch.
authors.forename: Alexander
authors.initials: A
authors.lastname: Schenk
authors.affiliation: Departments of Analytical Development, Max Zeller Söhne AG, Seeblickstrasse 4, CH 8590 Romanshorn, Switzerland.
authors.forename: Beate
authors.initials: B
authors.lastname: Siewert
authors.affiliation: Departments of Analytical Development, Max Zeller Söhne AG, Seeblickstrasse 4, CH 8590 Romanshorn, Switzerland.
authors.forename: Stephan
authors.initials: S
authors.lastname: Toff
authors.affiliation: Preclinical Research, Max Zeller Söhne AG, Seeblickstrasse 4, CH 8590 Romanshorn, Switzerland.
authors.forename: Jürgen
authors.initials: J
authors.lastname: Drewe
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D016014:Linear Models; D036901:Petasites / Q000737:chemistry*; D010936:Plant Extracts / Q000737:chemistry*; D011763:Pyrrolizidine Alkaloids / Q000032:analysis* / Q000737:chemistry; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D019032:Spectrometry, Mass, Matrix-Assisted Laser Desorption-Ionization / Q000379:methods*
chemical_list: D010936:Plant Extracts; D011763:Pyrrolizidine Alkaloids
keywords: Mass spectroscopy; Pyrrolizidine alkaloids; UPLC