Determination of Chlormequat and Mepiquat in Foods by Liquid Chromatography/Mass Spectrometry or Liquid Chromatography/Tandem Mass Spectrometry: Interlaboratory Study

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.