[Determination of ethychlozate and its degradation product in fruits by HPLC and LC/MS].
A method was developed for the analysis of ethychlozate (CIE) and its decomposition compound, 5-chloro-3(1H)-indazolylacetic acid (CIA) in fruits by HPLC and LC/MS. The sample was homogenized with 1 mol/L HC1, and CIE and CIA were extracted with 5 mol/L HCl and acetone. They were extracted from the acetone extract with diethylether-n-hexane (2:1). CIE was hydrolyzed to CIA with methanol-4 mol/L KOH (1:1). The solution was made acidic, and CIA was extracted with diethylether-n-hexane (2:1). The extract was cleaned up on a silica gel column. CIA was determined by HPLC-UV and LC/MS (Scan or SIR). Four fruits were spiked with CIE or CIA at 0.5 microgram/g and analyzed by the proposed method with HPLC. The average recoveries were 77.2-83.2% for CIE and 71.2-89.2% for CIA. The concentrations determined by LC/MS were 10-25% higher than the values by HPLC. The limit of detection (LOD) of CIA standard solution by HPLC corresponds to 0.015 microgram/g of CIE in the sample. In the same way, the LOD of CIA by LC/MS (SIR) corresponds to 0.009 microgram/g of CIE in the sample.
Takatsuki
Satoshi
S
National Institute of Health Sciences: 1-18-1, Kamiyoga, Setagaya-ku, Tokyo 158-8501, Japan.
Nemoto
Satoru
S
Sasaki
Kumiko
K
Toyoda
Masatake
M
D002851:Chromatography, High Pressure Liquid; D005638:Fruit / Q000737:chemistry*; D008401:Gas Chromatography-Mass Spectrometry; D006868:Hydrolysis; D007191:Indazoles / Q000032:analysis; D010937:Plant Growth Regulators / Q000032:analysis*
D007191:Indazoles; D010937:Plant Growth Regulators; C458560:ethychlozate