Determination of residues of the plant growth regulator chlormequat in pears by ion-exchange high performance liquid chromatography-electrospray mass spectrometry.
We report a method which we have used routinely for the determination of chlormequat residues in pears. After extraction with methanol, determination was performed, without clean-up, by ion-exchange HPLC using an SCX column eluted with aqueous ammonium formate-methanol, and HPLC-MS with an electrospray interface. MS and MS-MS were employed concurrently, using selected ion monitoring and selected reaction monitoring, respectively, of the 35Cl and 37Cl isotopes of the chlormequat cation and the CID transitions of each of these precursors to the common product ion at m/z 58. The method was suitable for determinations at concentrations of chlormequat cation of 0.04 mg kg-1. Concentrations determined using the four signals were in good agreement (mean RSD 3%). The mean recovery of chlormequat cation at 0.16 mg kg-1, measured using the m/z 122-->58 signal, was 86% (RSD 7%) under repeatability conditions and 88% (RSD 15%) in routine application of the method over a 3 month period. Analysis of an in-house reference sample of pears, similarly analysed over the 3 month period, gave an RSD of 10% with a mean of 0.14 mg kg-1. Mean recovery at 0.016 mg kg-1, under repeatability conditions on two occasions, was 101% (RSD 6%) and 56% (RSD 12%).
Startin
J R
JR
Central Science Laboratory, Sand Hutton, York, UK. j.startin@csl.gov.uk
Hird
S J
SJ
Sykes
M D
MD
Taylor
J C
JC
Hill
A R
AR
D002716:Chlormequat / Q000032:analysis*; D002851:Chromatography, High Pressure Liquid / Q000379:methods; D004350:Drug Residues / Q000032:analysis*; D005506:Food Contamination / Q000032:analysis*; D005638:Fruit / Q000737:chemistry*; D013058:Mass Spectrometry / Q000379:methods; D010937:Plant Growth Regulators / Q000032:analysis*
D010937:Plant Growth Regulators; D002716:Chlormequat