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牛乳中三氮脒残留高效液相色谱检测方法的建立 | |
其他题名 | Development of a high performance liquid chromatography method for the detection of diminazene diaceturate residue in milk |
刘瑾; 曾振灵; 余静贤; 刘戎; 李博; 赵吉祥; 陈红 | |
来源期刊 | 中国兽医科学
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ISSN | 1673-4696 |
出版年 | 2012 |
卷号 | 42期号:5页码:533-536 |
中文摘要 | 以乙腈沉淀牛乳中的蛋白质,上清液采用Oasis WCX固相萃取小柱净化浓缩,用乙酸-甲醇溶液洗脱药物,研究了牛乳中三氮脒残留的高效液相色谱检测方法。洗脱液上机检测,紫外检测波长372nm,色谱分析柱为氰基柱,流动相为V(乙腈)∶V(甲酸铵溶液)=10∶90,等度洗脱。当样品中三氮脒的含量为0.010~1.00mug/mL时,药物质量浓度与检测信号存在良好的相关性(r~2>0.999);牛乳中三氮脒的检测限为0.50*10~(-2)mug/mL,定量限为0.010mug/mL。牛乳按0.010、0.10和1.00mug/mL 3个添加水平做三氮脒的回收率试验,回收率≥82%,变异系数在1.3~4.2之间。结果表明,本研究建立的三氮脒残留高效液相色谱检测方法重复性好,灵敏度高,操作简便,可用于牛乳中三氮脒残留的检测。 |
英文摘要 | A high performance liquid chromatography(HPLC) method was developed for the determination of diminazene diaceturate in milk.Diminazene diaceturate was extracted with acetonitrile from milk.Oasis WCX cartridges was used to purify and concentrate the drug after centrifugation.The drug was then eluted by acetic acid-methanol.The sample was detected under the ultraviolet(UV) wavelength of 372 nm.Mobile phase consisted of acetonitrile and 0.02 mol/L ammonium formate solution(10∶90,V∶V) were used for isocratic elution and the flow rate was 1 mL/min.Within the range of 0.010 mug/mL to 1.00 mug/mL of diminazene diaceturate in milk,good linearity between drug concentration and detection signal was obtained(r~2>0.999).The limit of detection and limit of quantification of the examined diminazene diaceturate in milk were 0.5*10~(-2) mug/mL and 0.010 mug/mL for milk,respectively.The recoveries from spiked milk at three levels(0.010 mug/mL,0.10 mug/mL,and 1.00 mug/mL) were more than 82%,and the coefficient of variation ranged from 1.3 to 4.2.The developed method showed good reproducibility,high sensitive,expedience and could be applied to the determination of diminazene diaceturate in milk. |
中文关键词 | 牛乳 ; 三氮脒 ; 高效液相色谱-紫外检测法 |
英文关键词 | milk diminazene diaceturate HPLC-UV method |
语种 | 中文 |
国家 | 中国 |
收录类别 | CSCD |
WOS类目 | AGRICULTURE MULTIDISCIPLINARY |
WOS研究方向 | Agriculture |
CSCD记录号 | CSCD:4530856 |
资源类型 | 期刊论文 |
条目标识符 | http://119.78.100.177/qdio/handle/2XILL650/229106 |
作者单位 | 华南农业大学兽医学院, 国家兽药残留基准实验室, 广州, 广东 510642, 中国 |
推荐引用方式 GB/T 7714 | 刘瑾,曾振灵,余静贤,等. 牛乳中三氮脒残留高效液相色谱检测方法的建立[J],2012,42(5):533-536. |
APA | 刘瑾.,曾振灵.,余静贤.,刘戎.,李博.,...&陈红.(2012).牛乳中三氮脒残留高效液相色谱检测方法的建立.中国兽医科学,42(5),533-536. |
MLA | 刘瑾,et al."牛乳中三氮脒残留高效液相色谱检测方法的建立".中国兽医科学 42.5(2012):533-536. |
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