水、土中氟氯比之殘留分析

Analytical Methods for the Determination of Fluroxypyr Residues in Water and Soil

李貽華(Yi-Hwar Lee) ； 徐慈鴻(Tsyr-Horng Shyu)

《中華民國雜草學會會刊》 27卷1期 (2006/06) Pp. 31-42

https://doi.org/10.6274/WSSROC-2006-027(1)-031

摘要

本研究建立以氣相層析儀附電子捕獲式檢出器檢測水、土中氟氯比殘留量之方法。氟氯比推薦於防治柑桔園雜草，其在水、土中之殘留情形在台灣尚未被探討。水樣以二氯甲烷萃取，萃取液經脫水後濃縮至近乾，加甲醇及酸反應形成酯類衍生物，然後經過矽酸鎂淨化管除去雜質，收集淋洗液後濃縮並定量，注入氣相層析儀，使用電子捕獲式檢出器測定水樣中氟氯比之濃度。利用90%丙酮／0.1N鹽酸水溶液將土壤中之氟氯比抽取出，加甲醇及酸反應形成酯類衍生物，然後經過矽酸鎂淨化管除去雜質，收集淋洗液後濃縮並定量，以氣相層析儀附電子捕獲式檢出器檢測土壤中氟氯比之濃度。氟氯比之線性迴歸係數為0.981。分別添加3.4、6.7及13.3μg/L之標準品於水中進行回收率試驗，平均回收率為90.3~93.2%。分別添加0.16、0.20及0.24mg/Kg之標準品於土壤中進行回收率試驗，平均回收率分別為77.6~81.2%。水中之偵測界限為1.59μg/L，土中之測偵測界限為0.015mg/Kg，以建立之方法分析柑桔園土壤及柑桔園下方蓄水池水中之氟氯比殘留，結果皆未檢測出氟氯比。柑桔園使用之氟氯比污染水源之可能性低。

關鍵字

氟氯比 ； 殘留 ； 水 ； 土 ； 柑桔園

並列摘要

A precise method was developed for detecting the residues of fluroxypyr by gas liquid chromatography (GLC) with electron capture detector. Fluroxypyr is used for weed control in citrus orchard in Taiwan. The residues of fluroxypyr in water and soil have not been studied in Taiwan. The water sample is acidified with sulfuric acid and extracted with methylene chloride. The fluroxypyr in the extracts was methylated with methanol and sulfuric acid. After florisil column cleanup, the methylated fluroxypyr is determined by gas chromatograph equipped with an electron capture detector. Soil samples were extracted with 90% acetone in 0.1N HCl. The fluroxypyr in the extracts was methylated with methanol and sulfuric acid. After florisil column cleanup, the methylated fluroxypyr is determined by gas chromatograph equipped with an electron capture detector. The correlation coefficient of the linear standard curves of fluroxypyr was 0.981. Recoveries of fluroxypyr in water were in the 90.3-93.2% range. Recovery of fluroxypyr in soil was in the 77.6-81.2% range. The detection limit of fluroxypyr in water and soil were 1.59μg/L and 0.015 mg/Kg, respectively. This study was conducted to investigate the residues of water and soil following fluroxypyr application. Water samples collected from pond lower of the citrus orchard. No residue of fluroxypyr was detected in water and soils which were sampled from citrus orchard.

並列關鍵字

fluroxypyr ； residue ； water ； soil ； citrus orchard