分析化学
分析化學
분석화학
CHINESE JOURNAL OF ANALYTICAL CHEMISTRY
2014年
12期
1838-1841
,共4页
周茜%陈满堂%朱丽华%丁耀彬
週茜%陳滿堂%硃麗華%丁耀彬
주천%진만당%주려화%정요빈
高效液相色谱%电喷雾式检测器%在线固相萃取%红霉素%快速溶剂萃取
高效液相色譜%電噴霧式檢測器%在線固相萃取%紅黴素%快速溶劑萃取
고효액상색보%전분무식검측기%재선고상췌취%홍매소%쾌속용제췌취
High performance liquid chromatography%Corona-charged aerosol detector%Online solid phase extraction%Erythrocin%Accelerated solvent extraction
将在线固相萃取( online SPE)与高效液相色谱( HPLC)-通用型电喷雾检测器( CAD)结合,建立了集约养殖业常用抗生素红霉素的分析方法。5.0 g鸡粪样品与硅藻土混合后,置于34 mL萃取池中,以热水为萃取剂,在70℃、10.4 MPa条件下,用快速溶剂萃取仪提取样品中的红霉素。利用双三元液相色谱仪,采用在线富集进样方式,经Acclaim 120 C18色谱柱,以乙腈-0.1%甲酸溶液为流动相分离后,用CAD进行检测。红霉素在21~2000μg/kg范围内线性关系良好(r≥0.99),检出限为6.3μg/kg,加标回收率为79.2%~87.5%。
將在線固相萃取( online SPE)與高效液相色譜( HPLC)-通用型電噴霧檢測器( CAD)結閤,建立瞭集約養殖業常用抗生素紅黴素的分析方法。5.0 g鷄糞樣品與硅藻土混閤後,置于34 mL萃取池中,以熱水為萃取劑,在70℃、10.4 MPa條件下,用快速溶劑萃取儀提取樣品中的紅黴素。利用雙三元液相色譜儀,採用在線富集進樣方式,經Acclaim 120 C18色譜柱,以乙腈-0.1%甲痠溶液為流動相分離後,用CAD進行檢測。紅黴素在21~2000μg/kg範圍內線性關繫良好(r≥0.99),檢齣限為6.3μg/kg,加標迴收率為79.2%~87.5%。
장재선고상췌취( online SPE)여고효액상색보( HPLC)-통용형전분무검측기( CAD)결합,건립료집약양식업상용항생소홍매소적분석방법。5.0 g계분양품여규조토혼합후,치우34 mL췌취지중,이열수위췌취제,재70℃、10.4 MPa조건하,용쾌속용제췌취의제취양품중적홍매소。이용쌍삼원액상색보의,채용재선부집진양방식,경Acclaim 120 C18색보주,이을정-0.1%갑산용액위류동상분리후,용CAD진행검측。홍매소재21~2000μg/kg범위내선성관계량호(r≥0.99),검출한위6.3μg/kg,가표회수솔위79.2%~87.5%。
A novel HPLC-CAD method coupled with on-line solid phase extraction ( SPE ) for the determination of erythrocin which was widely used in livestock farming was developed. After mixed with diatomite, 5. 0 g manure sample was put into the cell and extracted with hot water at 70℃ and 10. 3 MPa. An on-line SPE methodology was applied to pre-treat the sample, and the sample was seperated on an Acclaim 120 C18 column and analyzed by corona CAD detector using acetonitrile and 0. 1% formic acid as mobile phase. Good linearity for erythrocin was obtained in the range of 21-2000 μg/kg. The detection limit was 6. 3 μg/kg. The average recoveries were 79. 2%-87. 5%.