Affiliation:
1. Federal Institute for Risk Assessment, D-14191 Berlin, Germany
2. Central Science Laboratory, Sand Hutton, York, YO41 1LZ, United Kingdom
Abstract
Abstract
Interlaboratory validation studies have been performed on 2 methods for the determination of chlormequat (CLQ) and mepiquat (MPQ). Both methods used identical extraction procedures and stable isotope internal standardization but differed in the use of liquid chromatography/mass spectrometry (LC/MS) or LC/tandem mass spectrometry (LC/MS/MS) for the determination, the amount of internal standard used, and the expected limit of detection. After addition of deuterated internal standards, CLQ and MPQ were extracted with methanol–water and determined by LC/MS or LC/MS/MS with positive electrospray ionization. Eight European laboratories participated in the LC/MS method study, analyzing mushroom, pear, wheat flour, and fruit puree with residues of CLQ in the range 0.040–1.19 mg/kg and of MPQ in the range 0.041–0.39 mg/kg. For CLQ, the Horwitz ratio (HoRat) values for individual test materials/levels were in the range 0.85–1.13 with amean of 1.00, showing good method performance. For MPQ, the Ho values for mushroom, pear (both levels), and wheat flour were in the range 0.83–0.94, again indicating good method performance. For the determination of MPQ in infant food (fruit puree) at 0.041 mg/kg, the Ho was 1.7 when a value of 0 reported by one participant was excluded. In the LC/MS/MS study, in which 11 laboratories participated, a separate sample set was analyzed with residues of CLQ in the range 0.007–1.03 mg/kg and of MPQ in the range 0.008–0.72 mg/kg. Ho values for CLQ were in the range 0.27–1.36 and for MPQ in the range 0.51–2.10, all corresponding to acceptable method performance.
Publisher
Oxford University Press (OUP)
Subject
Pharmacology,Agronomy and Crop Science,Environmental Chemistry,Food Science,Analytical Chemistry
Cited by
17 articles.
订阅此论文施引文献
订阅此论文施引文献,注册后可以免费订阅5篇论文的施引文献,订阅后可以查看论文全部施引文献