中国兽药杂志
中國獸藥雜誌
중국수약잡지
CHINESE JOURNAL OF VETERINARY DRUG
2012年
12期
36-39
,共4页
王彩娟%祝伟霞%杨冀州%孙转莲%张巨洲%张书胜
王綵娟%祝偉霞%楊冀州%孫轉蓮%張巨洲%張書勝
왕채연%축위하%양기주%손전련%장거주%장서성
硝基呋喃%固相支撑液液萃取%平行蒸发%高效液相色谱
硝基呋喃%固相支撐液液萃取%平行蒸髮%高效液相色譜
초기부남%고상지탱액액췌취%평행증발%고효액상색보
nitrofuran%solid - supported - liquid - liquid extraction%parallel evaporation%HPLC
建立了固相支撑液液萃取-平行蒸发技术用于快速净化多种饲料中的呋喃唑酮、呋喃它酮、呋喃西林和呋喃妥因。先用甲醇-磷酸盐缓冲溶液提取样品,再用硅藻土固相支撑液液萃取净化,然后用全自动平行蒸发技术浓缩,最后用高效液相色谱-二极管阵列在365nm波长下检测。实验对提取溶剂、净化方法、萃取时间、萃取体积和色谱分离等实验条件进行了优化。四种硝基呋喃原药在0.05~10Ixg/mL范围内线性相关系数大于0.9997,方法定量限为0.1mg/kg,0.1、0.2、1.0mg/kgZ个浓度水平的加标回收率为78.4%-105.3%,相对标准偏差为1.8%~7.2%。实际饲料样品分析结果表明,该技术简化了样品前处理,提高了操作自动化程度,测定结果准确度高,可用于批量饲料样品中硝基呋喃类原药的快速质量监控分析。
建立瞭固相支撐液液萃取-平行蒸髮技術用于快速淨化多種飼料中的呋喃唑酮、呋喃它酮、呋喃西林和呋喃妥因。先用甲醇-燐痠鹽緩遲溶液提取樣品,再用硅藻土固相支撐液液萃取淨化,然後用全自動平行蒸髮技術濃縮,最後用高效液相色譜-二極管陣列在365nm波長下檢測。實驗對提取溶劑、淨化方法、萃取時間、萃取體積和色譜分離等實驗條件進行瞭優化。四種硝基呋喃原藥在0.05~10Ixg/mL範圍內線性相關繫數大于0.9997,方法定量限為0.1mg/kg,0.1、0.2、1.0mg/kgZ箇濃度水平的加標迴收率為78.4%-105.3%,相對標準偏差為1.8%~7.2%。實際飼料樣品分析結果錶明,該技術簡化瞭樣品前處理,提高瞭操作自動化程度,測定結果準確度高,可用于批量飼料樣品中硝基呋喃類原藥的快速質量鑑控分析。
건립료고상지탱액액췌취-평행증발기술용우쾌속정화다충사료중적부남서동、부남타동、부남서림화부남타인。선용갑순-린산염완충용액제취양품,재용규조토고상지탱액액췌취정화,연후용전자동평행증발기술농축,최후용고효액상색보-이겁관진렬재365nm파장하검측。실험대제취용제、정화방법、췌취시간、췌취체적화색보분리등실험조건진행료우화。사충초기부남원약재0.05~10Ixg/mL범위내선성상관계수대우0.9997,방법정량한위0.1mg/kg,0.1、0.2、1.0mg/kgZ개농도수평적가표회수솔위78.4%-105.3%,상대표준편차위1.8%~7.2%。실제사료양품분석결과표명,해기술간화료양품전처리,제고료조작자동화정도,측정결과준학도고,가용우비량사료양품중초기부남류원약적쾌속질량감공분석。
A rapid purification method was established for simultaneous determination of furazolidone, furan ketones, nitrofurazone and nitrofurantoin in feed using solid - supported - liquid - liquid extraction and parallel evaporation. The samples were extracted with methanol -phosphate buffer. The purification procedure was used with solid- supported- liquid- liquid extraction (SSLLE) and the concentration was selected with an automatic method of parallel evaporation (PE). The detection was performed by HPLC with diode - array detector (DAD) under 365 nm. The experimental parameters including extraction solvent, purification, extract time, extraction volumes, separation conditions were optimized. With the optimal conditions, the linear range of analytes was from 0.05 to 10 txg/mL with relative correlations more than 0.9997. The limit of quantification of the method was 0.1mg/kg. Spiked with 0.1,0.2 and 1 mg/kg, the recoveries were obtained from 78.4% to 105.3% with the relative standard deviation from 1.8% to 7.2%. The results of real feeds samples indicated that the method was simple, automatic, accurate, and can be used for quick quality monitoring analysis of batch feeds.