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歐索林酸於石斑魚與黑鯛之殘留試驗
友善列印
作者: 詹勳隆、林秋華、林文華、李淑慧
中文摘要: 本研究目的在於建立歐索林酸藥物殘留試驗並推算出石斑魚及黑鯛之停藥期,以供作水產動物用藥新增藥品及使用規範檢討參考依據。參照衛福部公告試驗方法,以電灑離子源正離子採用多重反應監測(MRM)模式下,超高效液相層析串聯質譜法分析歐索林酸於組織中殘留量。在分析條件下,其檢量線線性範圍為5-1000 μg/L,線性迴歸係數(R2)為0.9972,而偵測極限為3 μg/L,定量極限為5 μg/L;回收率以添加10-100 μg/kg進行評估,石斑魚肌肉(含皮)回收率介於79.0-81.4%,而肝臟添加回收率介於82.6-88.5%,黑鯛肌肉(含皮)回收率介於84.8-92.6%,肝臟添加回收率介於91.8-99.3%。石斑魚於肌肉(含皮)添加10-100 μg/kg濃度日內、日間精密度RSD分別介於3.8-9.2%與5.4-8.5%,肝臟日內、日間精密度RSD分別介於1.5-3.2 %及2.3-6.4%;黑鯛於肌肉(含皮)日內、日間精密度RSD分別介於1.4-5.2%與4.2-5.6%,肝臟日內、日間精密度RSD分別介於1.5-2.5%及2.2-3.2%。殘留試驗以歐索林酸低、高劑量30、60 mg/kg連續投予5天後,分別於1、3、5、7、10、14、21天等採樣,檢測其肌肉(含皮)、肝臟殘留之歐索林酸濃度。石斑魚及黑鯛低、高劑量組肌肉(含皮)、肝臟於投藥後分別於第10天及第5天殘留濃度均低於方法偵測極限。故以檢測不到殘留的時間再加上二分之一的安全期間即為停藥期,建議本藥物於石斑魚停藥期為15天,而黑鯛停藥期為8天。
英文摘要: The purpose of this study is to assess Oxolinic acid residues in grouper (Epinephelus coioides) and black seabream (Acanthopagrus schlegelii) and generate a basis for setting withdrawal periods, which could be used for reference in regulating newly approved aquatic animal drugs and usage policies. Based on the test methods announced by the Ministry of Health and Welfare, residues of Oxolinic acid in fish tissue was analyzed by ultra-performance liquid chromatography combined with electrospray ionization triple quadrupole tandem mass spectrometry (UPLC–MS/MS) under the multiple reaction monitoring (MRM) mode. Under the optimal conditions, the linear range was 5-1000 μg/L, the results showed a good linear relationship (R2= 0.9972). The limit of detection (LOD) was 3 μg/L and the limit of quantitation was 5 μg/L. The spiked levels were 10, 50, 100 μg/kg. The average recoveries of spiked test in grouper were 79.0-81.4 % in muscle with skin and 82.6-88.5 % in liver. The spiked test in black seabream, the average recoveries were 84.8-92.6 % in muscle with skin and 91.8-99.3 % in liver. The intra-assay of the muscle (with skin) and liver relative standard deviation (RSD) in grouper was 3.8-9.2 % and 5.4-8.5 % respectively, and the inter-assay was 1.5-3.2 % and 2.3-6.4 %. The intra-assay of the muscle (with skin) and liver RSD in black seabream was 1.4-5.2 % and 4.2-5.6 % respectively, and the inter-assay was 1.5-2.5 % and 2.2-3.2 %, respectively. The residual test was administered orally into two doses 30 and 60 mg/kg, for five consecutive days. The samples were collected at 1st, 3rd, 5th, 7th, 10th, 14th and 21st day,. The results showed that the residue levels in the muscles and livers with low and high doses were both under the method detection limit (3 μg/kg) on the 5th day in black seabream and the 10th day in groupers. Therefore, the withdrawal time is estimated to be 8 days in black seabream and 15 days in groupers.
備註: 年份:西元 2016 年
期別:第 50 期
詳細內容:
本研究目的在於建立歐索林酸藥物殘留試驗並推算出石斑魚及黑鯛之停藥期,以供作水產動物用藥新增藥品及使用規範檢討參考依據。參照衛福部公告試驗方法,以電灑離子源正離子採用多重反應監測(MRM)模式下,超高效液相層析串聯質譜法分析歐索林酸於組織中殘留量。在分析條件下,其檢量線線性範圍為5-1000 μg/L,線性迴歸係數(R2)為0.9972,而偵測極限為3 μg/L,定量極限為5 μg/L;回收率以添加10-100 μg/kg進行評估,石斑魚肌肉(含皮)回收率介於79.0-81.4%,而肝臟添加回收率介於82.6-88.5%,黑鯛肌肉(含皮)回收率介於84.8-92.6%,肝臟添加回收率介於91.8-99.3%。石斑魚於肌肉(含皮)添加10-100 μg/kg濃度日內、日間精密度RSD分別介於3.8-9.2%與5.4-8.5%,肝臟日內、日間精密度RSD分別介於1.5-3.2 %及2.3-6.4%;黑鯛於肌肉(含皮)日內、日間精密度RSD分別介於1.4-5.2%與4.2-5.6%,肝臟日內、日間精密度RSD分別介於1.5-2.5%及2.2-3.2%。殘留試驗以歐索林酸低、高劑量30、60 mg/kg連續投予5天後,分別於1、3、5、7、10、14、21天等採樣,檢測其肌肉(含皮)、肝臟殘留之歐索林酸濃度。石斑魚及黑鯛低、高劑量組肌肉(含皮)、肝臟於投藥後分別於第10天及第5天殘留濃度均低於方法偵測極限。故以檢測不到殘留的時間再加上二分之一的安全期間即為停藥期,建議本藥物於石斑魚停藥期為15天,而黑鯛停藥期為8天。
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