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J.Health Sci., 48(4), 335-340, 2002

Simultaneous Determination of Azimsulfuron, Flazasulfuron and Halosulfuron-methyl in Grains, Seeds, Vegetables and Fruits by HPLC

Susumu Ishimitsu,* Akiko Kaihara, Kimihiko Yoshii, Yukari Tsumura, Yumiko Nakamura, and Yasuhide Tonogai

National Institute of Health Sciences, Osaka Branch, Division of Food Chemistry, 1-1-43 Hoenzaka, Chuo-ku, Osaka 540-0006, Japan

A method was developed for the simultaneous determination of 3 sulfonylurea herbicides, azimsulfuron, flazasulfuron and halosulfuron-methyl in agricultural products. The herbicides were extracted with acetone, re-extracted with ethyl acetate, and then transferred to 2% dipotassium hydrogenphosphate solution. The herbicides were extracted again into ethyl acetate and cleaned up using Sep-Pak® Plus Alumina N and Bond Elut® SAX cartridge columns. The 3 sulfonylurea herbicides were determined by HPLC. The fortified peaks were confirmed by LC/MS with electrospray ionization (ESI), and the peaks of azimsulfuron, flazasulfuron and halosulfuron-methyl were determined. The recoveries of the 3 sulfonylurea herbicides from brown rice, corn, cotton seed, ginkgonut, chestnut, almond, walnut, cucumber, pumpkin, orange, grapefruit, mandarin, lemon and grape ranged from 77.0 to 112.3% following fortification at 0.05-0.5 mu g/g. The detection limits were 0.01 mu g/g for azimsulfuron and halosulfuron-methyl, and 0.02 mu g/ml for flazasulfuron(S/N > 3).