分析化学
分析化學
분석화학
CHINESE JOURNAL OF ANALYTICAL CHEMISTRY
2015年
9期
1285-1290
,共6页
章蕾%袁东星%方锴%刘宝敏
章蕾%袁東星%方鍇%劉寶敏
장뢰%원동성%방개%류보민
铁载体%固相萃取%高效液相色谱-串联质谱%海水
鐵載體%固相萃取%高效液相色譜-串聯質譜%海水
철재체%고상췌취%고효액상색보-천련질보%해수
Siderophore%Analysis%Solid phase extraction%Liquid chromatography-tandem mass spectrometry%Seawater
铁载体是一种由海洋菌类合成并分泌、能特异性络合海水中铁的有机配体。本研究建立了固相萃取预处理、高效液相色谱-串联质谱测定海水中铁载体化合物的分析方法。海水样品经0.22μm滤膜过滤,其中铁载体由ENVI-18萃取柱萃取、甲醇洗脱后得到富集净化后的试样;采用SB-C18反向色谱柱以0.1%( V/V)甲酸溶液和甲醇溶液梯度洗脱分离,在质谱的多反应监测正离子模式下检测。3种铁载体化合物标准物质Pyover-dines-Fe, Ferrichrome, Ferrioxamine E 的检测线性范围分别为0.001~3.0μg/mL,0.005~15.0μg/mL,0.001~3.0μg/mL,相关系数R2>0.99;仪器检出限分别为0.08,1.76和1.36 ng/mL;定量限分别0.27,5.87和4.53 ng/mL。在海水样品中添加铁载体化合物混合标准溶液,3种目标物测定值的相对标准偏差<12%,方法回收率分别为Pyoverdines-Fe 12.1%~18.6%,Ferrichrome 82.0%~97.7%,Ferrioxamine E 70.0%~98.3%。
鐵載體是一種由海洋菌類閤成併分泌、能特異性絡閤海水中鐵的有機配體。本研究建立瞭固相萃取預處理、高效液相色譜-串聯質譜測定海水中鐵載體化閤物的分析方法。海水樣品經0.22μm濾膜過濾,其中鐵載體由ENVI-18萃取柱萃取、甲醇洗脫後得到富集淨化後的試樣;採用SB-C18反嚮色譜柱以0.1%( V/V)甲痠溶液和甲醇溶液梯度洗脫分離,在質譜的多反應鑑測正離子模式下檢測。3種鐵載體化閤物標準物質Pyover-dines-Fe, Ferrichrome, Ferrioxamine E 的檢測線性範圍分彆為0.001~3.0μg/mL,0.005~15.0μg/mL,0.001~3.0μg/mL,相關繫數R2>0.99;儀器檢齣限分彆為0.08,1.76和1.36 ng/mL;定量限分彆0.27,5.87和4.53 ng/mL。在海水樣品中添加鐵載體化閤物混閤標準溶液,3種目標物測定值的相對標準偏差<12%,方法迴收率分彆為Pyoverdines-Fe 12.1%~18.6%,Ferrichrome 82.0%~97.7%,Ferrioxamine E 70.0%~98.3%。
철재체시일충유해양균류합성병분비、능특이성락합해수중철적유궤배체。본연구건립료고상췌취예처리、고효액상색보-천련질보측정해수중철재체화합물적분석방법。해수양품경0.22μm려막과려,기중철재체유ENVI-18췌취주췌취、갑순세탈후득도부집정화후적시양;채용SB-C18반향색보주이0.1%( V/V)갑산용액화갑순용액제도세탈분리,재질보적다반응감측정리자모식하검측。3충철재체화합물표준물질Pyover-dines-Fe, Ferrichrome, Ferrioxamine E 적검측선성범위분별위0.001~3.0μg/mL,0.005~15.0μg/mL,0.001~3.0μg/mL,상관계수R2>0.99;의기검출한분별위0.08,1.76화1.36 ng/mL;정량한분별0.27,5.87화4.53 ng/mL。재해수양품중첨가철재체화합물혼합표준용액,3충목표물측정치적상대표준편차<12%,방법회수솔분별위Pyoverdines-Fe 12.1%~18.6%,Ferrichrome 82.0%~97.7%,Ferrioxamine E 70.0%~98.3%。
Siderophores were produced and secreted with marine microorganisms as the highly specific iron chelators. A method of liquid chromatography-tandem mass spectrometric detection coupled with solid phase extraction pretreatment was developed for the determination of siderophores in seawater. The samples were filtered through a 0. 22 μm membrane, extracted with an ENVI-18 cartridge and then eluted with methanol. The separation of the analytes was performed on a reversed phase SB-C18 column with a gradient elution program by using 0. 1% ( V/V) formic acid and methanol as the mobile phases. Qualitative analysis was performed in multiple-reaction monitoring mode. Good linearity (R2>0. 99) was obtained for Pyoverdines-Fe, Ferrichrome, Ferrioxamine E at the concentrations of 0. 001-3. 00 μg/mL, 0. 005-15. 00 μg/mL, 0. 001-3. 00 μg/mL, respectively. The instrumental detection limits and limits of quantification for the three analytes were 0. 08, 1. 76 and 1. 36 ng/mL; 0. 27, 5. 87 and 4. 53 ng/mL, respectively. The relative standard deviations were lower than 12%, while the recoveries were 12. 1%-18. 6% for Pyoverdines-Fe, 82. 0%-97. 7% for Ferrichrome, and 70. 0%-98. 3% for Ferrioxamine E.