畜水產品中歐索林酸及乃託文檢方法之探討及其殘留量之調查

Analytical Methods of Oxolinic Acid and Nitrovin and Residues in Livestock and Fishery Products

饒麥玲(Mai-Ling Jao) ； 施養志(Yang-Chih Shih) ； 張碧秋(Pi-Chih Chang) ； 李乾鐘(Cuan-Chung Li)

《藥物食品檢驗局調查研究年報》 9號 (1991/09) Pp. 289-298

https://doi.org/10.6946/ASRNL.199109.0289

摘要

本研究以快速，簡便的高效液相層析法(High Performance Liquid Chromatography)對畜水產品中的抗菌劑－歐索林酸(Oxolinic acid)及乃託文(Nitrovin)之檢驗法進行探討，並調查市售或外銷之蝦類，鰻魚，豬肉，牛肉等檢體中歐索林酸及乃託文之殘留量，以確保國人之健康及維護外銷信譽。歐索林酸之檢驗方法是將檢體以二氣甲烷萃取、濃縮後，以正己烷去脂肪，再經二氯甲烷抽取濃縮後之殘留物，以重氮甲烷(Diazomethane)甲基化一小時，利用高效液相層析儀分析。以此法所得之最低檢測限量為50ppb。而分別添加歐索林酸0.3、1及2μg等三種量於四種不同之檢體中，其回收率為88.2~96.9%。變異系數是1.4~6.3%。抽購市售90件檢體，檢測其歐索林酸之殘留量，檢出七件，檢出率為7.7%，殘留量範圍在65~72ppb之間。
乃託文(Nitrovin)。檢體經丙酮的萃取、濃縮後，以正己烷去脂肪，再以氯仿分配分層萃取，氯仿層濃縮至乾，殘留物以85%乙腈溶解通過Alumina SEP PAK，再以高效液相層析儀分析，添如不同量乃託文(1、5μg)於檢體之回收率為80.1~92.3%，變異係數是1.7~6.1%，最低檢出限量為20ppb，抽購市售雞肉及堵肉20件，檢測其乃託文之殘留量，均未檢出。

關鍵字

高效液相層析儀 ； 畜水產品 ； 抗菌劑 ； 歐索林酸 ； 乃託文 ； 甲基化

並列摘要

A simple, rapid high performance liquid chromatography (HPLC) method was described for the determination of oxolinic acid and its residues in livestock and fishery products. Five g of sample was extracted from meats by dichloromethane, removed lipids by n-hexane, then methylated by d-azomethane. The filtrate was subjected to HPLC with UV detector at 254nm. Separation was achieved by using Methanol HO (60:40) on Licrospher 100RP-18 column and flow rate 0.6m1/min. Oxolinic acid was found to have a retention time of about 5.2 minutes Recoveries (C.V%) of three different levels (0.3、 1 and 2μg) were 88.2-96.9% (1.4-6.3%). The detection limit was 50ppb.
For determination of nitrovin and its residues in livestock and fishery products, a simple rapid high performance liquid chromatography (HPLC) method was developed. Ten g of sample was extracted from meats by aceton, removed lipids by n-hexene, and partitioned with chloroform, cleaned up by Alumina B SEP PAK. The filtrate was subjected to HPLC with UV detector at 380nm, Separation was achieved by using Acetonitrile Acetic acid: H2O (70:0.1:30) on μ Bondapak C81 column and flow rate 0.6m1/min. Nitovin was found to have a retention time of about 6.5 minutes. Recoveries (C.V%) of three different levels (15 and l0μg) were 80.1~92.3% (1.7~6.1%). The detection limit was 20ppb.