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饲料中硝基呋喃类药物高效液相色谱检测方法的建立
王蕾, 鲍恩东
0
(南京农业大学 动物医学院,南京 210095)
摘要:
为检测饲料中硝基呋喃类药物,建立呋喃西林、呋喃妥因、呋喃唑酮和呋喃他酮4种硝基呋喃类药物检测的高效液相色谱法。采用乙腈提取饲料中4种呋喃类药物,将提取液浓缩后用上样液溶解残渣,经过HLB固相萃取柱净化后,以乙腈-乙酸铵溶液为流动相,反相色谱柱分离,在Waters Sunfire C18色谱柱上,紫外检测器365 nm 波长下分离检测,外标法定量。结果表明:4种硝基呋喃类药物的标准曲线回归系数均在0.999 7以上,线性范围在0.2~30.0 μg/mL;不同添加浓度的加标回收率≥70%~98%,回收率标准偏差≤10%;呋喃西林、呋喃妥因、呋喃唑酮和呋喃它酮的检测限依次为0.020、0.020、0.020和0.100 μg/mL;定量限依次为0.50、0.50、0.50 和1.00 mg/kg。本试验建立的高效液相色谱法具有操作相对简单,线性范围良好,且重复性好的特点,且适于配合饲料、浓缩饲料和预混合饲料中硝基呋喃类药物的检测。
关键词:  饲料  高效液相色谱法  固相萃取  呋喃类药物
DOI:10.11841/j.issn.1007-4333.2011.02.020
投稿时间:2010-08-31
基金项目:农业部农业行业标准制定项目(农财发[2009]105号-50)
Establishment of HPLC method for determinationof nitrofurans in feeds
WANG Lei, BAO En-dong
(College of Veterinary Medicine,Nanjing Agricultural University,Nanjing 210095,China)
Abstract:
To detect nitrofurans in feeds,a high performance liquid chromatography (HPLC) method for determination of nitrofurans,such as Furacillin,Nitrofurantion,Furazolidone,and Furaltadone,was established in this study.Nitrofurans in feeds was extracted by acetonitrle,concentrated extraction was cleaned up with HLB solid phase extraction (SPE) column.Nitrofurans were separated on Water Sunfire C18 column with UV detector 365 nm,using acetonitrile and ammonium acetate buffer as mobile phase.The results showed that the nitrofurans standard curve regression coefficient is above 0.9997,and the linearity range is 0.2~30.0 μg/mL.The average recoveries of nitrofurans ranged from 70%~98%,with RSD below 10%.The detection limit of Furacillin,Nitrofurantion,Furazolidone and Furaltadone was 0.020,0.020,0.020 and 0.100 μg/mL,respectively;and the quantitation limit was 0.50,0.50,0.50 and 1.00 mg/kg,respectively.This method exhibits uncomplicated operation,excellent linearity,high sensitivity and superior reproducibility for determination of nitrofurans residues in formula feed,concent-rate feed and premixes feed.
Key words:  feeds  HPLC  solid-phase extraction  nitrofurans