摘要
研究旨在建立一种检测水产饲料中复方硝基酚钠含量的高效液相色谱方法。饲料经乙腈提取,正己烷液液萃取净化,无水硫酸钠脱水,碱性条件下浓缩后,以0.1%磷酸溶液-甲醇溶液（体积比63？？37）为流动相,经C18色谱柱分离,紫外检测波长280 nm下分离检测。结果表明,对硝基酚钠、邻硝基酚钠和5-硝基邻甲氧基苯酚钠的检出限均为0.5 mg/kg,定量限均为1.0 mg/kg。该方法在0.5~20μg/ml范围内线性关系良好,相关系数r2〉0.999。添加水平为1~20 mg/kg时,对硝基酚钠、邻硝基酚钠和5-硝基邻甲氧基苯酚钠的回收率分别为84.5%~96.6%、74.0%~89.2%和78.5%~95.8%,批内相对标准偏差及批间相对标准偏差均〈15%。经验证该方法操作简便,准确性和重现性良好,可用于水产饲料中复方硝基酚钠含量的测定。
This study aimed to establish a kind of HPLC method of detecting compound sodium nitro-phenolates in aquatic feeds. The samples were extracted by acetonitrile. The extracts were purified byliquid- liquid extraction with n- hexane and dehydrated by anhydrous sodium sulfate. Then the ex-tracts were concentrated in alkaline conditions. The analytes were separated on C18 column with UVdetector at 280 nm, using 0.1% phosphoric acid solution and methanol（V？？ V=63？？ 37） as mobilephase. The result showed that, the detection limits of ρ-nitrophenol sodium, ο-nitrophenol sodiumand 2-methoxy-5-nitropenolate sodium were 0.5 mg/kg, and the quantification limits were 1.0 mg/kg,respectively. In the range of 0.5~20 μg/ml, there was a good linear correlation（r20.999） between thepeak area and concentration of ρ-nitrophenol sodium, ο-nitrophenol sodium and 2-methoxy-5-nitro-penolate sodium. The average recoveries for aquatic feeds samples of ρ-nitrophenol sodium, ο-nitro-phenol sodium and 2-methoxy-5-nitropenolate sodium were 84.5%~96.6%, 74.0%~89.2% and 78.5%~95.8%, respectively, with the intra and inter batch relative standard deviation were less than 15%.The method was tested to be of convenience, high sensitivity, good accuracy and precision, and it issuitable for determination of compound sodium nitrophenolates in aquatic feeds.
出处
《饲料工业》
北大核心
2015年第12期53-57,共5页
Feed Industry
基金
2014年国家水产品质量安全风险评估项目[GJFP2014009]
"十二五"国家科技支撑计划项目[2012BAD29B06]
