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ANALYTICAL INSTRUMENTATION
2015年
4期
14-18
,共5页
冯晓青%刘华良%阮丽萍%王芹%王露%汪怡%杭学宇
馮曉青%劉華良%阮麗萍%王芹%王露%汪怡%杭學宇
풍효청%류화량%원려평%왕근%왕로%왕이%항학우
酸性橙Ⅱ%黄鱼%HPLC
痠性橙Ⅱ%黃魚%HPLC
산성등Ⅱ%황어%HPLC
acid orangeⅡ%yellow croaker%HPLC
建立了操作简便、灵敏度较高的HPLC测定黄鱼中酸性橙Ⅱ的方法。样品经均质,取2 g粉碎样品,乙醇震荡提取5 min ,提取液经聚酰胺固相萃取柱分离净化,采用C18色谱柱(250 mm ×4.6 mm ×5μm )分离,以甲醇‐乙酸铵溶液梯度洗脱,流速为1 mL/min ,设定柱温30℃,进样体积为10μL ,二极管阵列检测器在λ=485 nm处检测酸性橙Ⅱ(λ=485 nm)。酸性橙Ⅱ在0.1μg/mL~20μg/mL的范围内,呈良好的线性响应,线性方程为 y=34.94x-2.697,r=0.9998。酸性橙Ⅱ检出限为0.08μg/mL。样品添加浓度为0.5 mg/kg~15 mg/kg时,方法回收率为96%~99%,相对标准偏差为3.4%~7.3%。该法用于黄鱼中的酸性橙Ⅱ的含量测定,操作简便,定量准确可靠。
建立瞭操作簡便、靈敏度較高的HPLC測定黃魚中痠性橙Ⅱ的方法。樣品經均質,取2 g粉碎樣品,乙醇震盪提取5 min ,提取液經聚酰胺固相萃取柱分離淨化,採用C18色譜柱(250 mm ×4.6 mm ×5μm )分離,以甲醇‐乙痠銨溶液梯度洗脫,流速為1 mL/min ,設定柱溫30℃,進樣體積為10μL ,二極管陣列檢測器在λ=485 nm處檢測痠性橙Ⅱ(λ=485 nm)。痠性橙Ⅱ在0.1μg/mL~20μg/mL的範圍內,呈良好的線性響應,線性方程為 y=34.94x-2.697,r=0.9998。痠性橙Ⅱ檢齣限為0.08μg/mL。樣品添加濃度為0.5 mg/kg~15 mg/kg時,方法迴收率為96%~99%,相對標準偏差為3.4%~7.3%。該法用于黃魚中的痠性橙Ⅱ的含量測定,操作簡便,定量準確可靠。
건립료조작간편、령민도교고적HPLC측정황어중산성등Ⅱ적방법。양품경균질,취2 g분쇄양품,을순진탕제취5 min ,제취액경취선알고상췌취주분리정화,채용C18색보주(250 mm ×4.6 mm ×5μm )분리,이갑순‐을산안용액제도세탈,류속위1 mL/min ,설정주온30℃,진양체적위10μL ,이겁관진렬검측기재λ=485 nm처검측산성등Ⅱ(λ=485 nm)。산성등Ⅱ재0.1μg/mL~20μg/mL적범위내,정량호적선성향응,선성방정위 y=34.94x-2.697,r=0.9998。산성등Ⅱ검출한위0.08μg/mL。양품첨가농도위0.5 mg/kg~15 mg/kg시,방법회수솔위96%~99%,상대표준편차위3.4%~7.3%。해법용우황어중적산성등Ⅱ적함량측정,조작간편,정량준학가고。
A method for determination of acid orange Ⅱ in yellow croaker ,was developed.Samples were homogenized ,2 grams of sample were extracted with ethanol for 5 minutes. The extract was separa‐ted and purified by polyamide solid phase extraction column. The HPLC separation was achieved by using C18(250 mm × 4.6 mm ,5μm) with a mobile phase consisting of methanol and acetate buffer ,and the gra‐dient program was used at a flow rate of 1 ml/min. The column temperature was set at 30 ℃ and the injec‐tion volume was 10 μl. The detection wavelength was at 485 nm for acid orangeⅡ ,then we selected the best chromatograph conditions to determine the concentration of acid orangeⅡ in yellow croaker and its added standard recoveries. This method exhibited a linear relation within 0.1 20 μg/ml acid orangeⅡcontent. The regression equation was y=34.94x2.697 ( r=0.9998) and the minimum detectable limit of this method was 0.08μg/ml. The recoveries were 96%‐99% ,the relative standard deviations(RSDs) were 3.39% 7.31% while the contents of added standard were 0.5 10 mg/kg. The method is simple ,accurate and reliable .