N. Takeda et al., HPLC ANALYSIS OF PESTICIDES IN BROWN RICE USING UV ABSORPTION AND POSTCOLUMN PHOTOLYSIS-FLUORESCENCE DETECTION, Shokuhin Eiseigaku Zasshi, 36(5), 1995, pp. 601-606
A simple and selective HPLC method was developed for the systematic de
termination of bentazone (BEN), imazaril (IMZ), inabenfide (INA), pyra
zoxyfen (PYR) and chinomethionate (CIN) in imported brown rice. A rice
sample was extracted with 70% MeCN and divided into three fractions (
acidic, BEN; basic, IMZ/INA; neutral, PYR/CIN). The acidic and basic f
ractions were purified by partition between n-hexane-dichloromethane (
1:1) and either 0.01 M berate buffer (pH 10.4) for BEN or 0.1 M HCl fo
r IMZ/INA, immediately before injection into the HPLC system. The PYR/
CIN fraction was redissolved in isopropanol-MeCN (1:1) to remove lipid
components. A sample was analyzed on an ODS column with a mobile phas
e of a mixture of MeCN-5 mM K2HPO4 [BEN: (20:80), pH 2.5; IMZ/INA: (35
: 65), pH 4.5; PYR/CIN: (55 :45)] at 45 degrees C. IMZ and INA were d
etermined from the UV absorption at 220 nm. Other pesticides were dete
rmined by using a postcolumn photolysis-fluorescence detection system
at an excitation wavelength (Ex) of 329 nm and emission wavelength (Em
) of 415 nm for BEN, Ex 333 nm/Em 405 nm for PYR, and Ex 377 nm/Em 450
nm for CIN. Average recoveries ranged from 80.9 to 89.1% at a fortifi
cation level of 0.025 mu g/g. The limit of determination was 0.005 mu
g/g for INA and 0.01 mu g/g for other pesticides. The method was appli
ed to 24 brown rice samples, and all appeared to be free from the five
pesticides.