分析化学
分析化學
분석화학
CHINESE JOURNAL OF ANALYTICAL CHEMISTRY
2012年
7期
1002-1010
,共9页
许志刚%杜卓%胡玉玲%胡玉斐%潘英朋%李攻科
許誌剛%杜卓%鬍玉玲%鬍玉斐%潘英朋%李攻科
허지강%두탁%호옥령%호옥비%반영붕%리공과
分子印迹聚合物%吸附萃取搅拌棒%甲氧苄啶%磺胺药物%复杂样品
分子印跡聚閤物%吸附萃取攪拌棒%甲氧芐啶%磺胺藥物%複雜樣品
분자인적취합물%흡부췌취교반봉%갑양변정%광알약물%복잡양품
Molecularly imprinted polymer%Stir bar sorptive extraction%Trimethoprim%Sulfonamides%Complex sample
研制了甲氧苄啶分子印迹吸附萃取搅拌棒涂层,并应用于复杂样品中痕量甲氧苄啶和磺胺药物的分析.分子印迹涂层的厚度约为21.5μm,相对标准偏差为5.9％(n=10),涂层均匀、致密,具有良好的热稳定性和化学稳定性.分子印迹涂层的萃取容量是非印迹涂层萃取容量的1.7倍,分子印迹涂层对抗菌增效剂、磺胺药物、三嗪化合物和甲氨蝶呤都表现出良好的选择性吸附萃取能力.建立了分子印迹吸附萃取搅拌棒联用高效液相色谱的分析方法,成功应用于加标尿样和血浆中痕量甲氧苄啶的分析,线性范围为5 ～ 200μg/L,检出限为1.6μg/L,在尿样和血浆中的回收率范围分别为84.5％～91.7％和71.9％～85.1％,标准偏差分别为29％～4 4％和3.0％～7.3％.该方法还应用于加标牛奶中痕量磺胺药物的分析,线性范围为10～200μg/L,检出限在4.5～6.1 μg/L之间,回收率为83.2％～110.2％,标准偏差为4.1％～8.0％.
研製瞭甲氧芐啶分子印跡吸附萃取攪拌棒塗層,併應用于複雜樣品中痕量甲氧芐啶和磺胺藥物的分析.分子印跡塗層的厚度約為21.5μm,相對標準偏差為5.9％(n=10),塗層均勻、緻密,具有良好的熱穩定性和化學穩定性.分子印跡塗層的萃取容量是非印跡塗層萃取容量的1.7倍,分子印跡塗層對抗菌增效劑、磺胺藥物、三嗪化閤物和甲氨蝶呤都錶現齣良好的選擇性吸附萃取能力.建立瞭分子印跡吸附萃取攪拌棒聯用高效液相色譜的分析方法,成功應用于加標尿樣和血漿中痕量甲氧芐啶的分析,線性範圍為5 ～ 200μg/L,檢齣限為1.6μg/L,在尿樣和血漿中的迴收率範圍分彆為84.5％～91.7％和71.9％～85.1％,標準偏差分彆為29％～4 4％和3.0％～7.3％.該方法還應用于加標牛奶中痕量磺胺藥物的分析,線性範圍為10～200μg/L,檢齣限在4.5～6.1 μg/L之間,迴收率為83.2％～110.2％,標準偏差為4.1％～8.0％.
연제료갑양변정분자인적흡부췌취교반봉도층,병응용우복잡양품중흔량갑양변정화광알약물적분석.분자인적도층적후도약위21.5μm,상대표준편차위5.9％(n=10),도층균균、치밀,구유량호적열은정성화화학은정성.분자인적도층적췌취용량시비인적도층췌취용량적1.7배,분자인적도층대항균증효제、광알약물、삼진화합물화갑안접령도표현출량호적선택성흡부췌취능력.건립료분자인적흡부췌취교반봉련용고효액상색보적분석방법,성공응용우가표뇨양화혈장중흔량갑양변정적분석,선성범위위5 ～ 200μg/L,검출한위1.6μg/L,재뇨양화혈장중적회수솔범위분별위84.5％～91.7％화71.9％～85.1％,표준편차분별위29％～4 4％화3.0％～7.3％.해방법환응용우가표우내중흔량광알약물적분석,선성범위위10～200μg/L,검출한재4.5～6.1 μg/L지간,회수솔위83.2％～110.2％,표준편차위4.1％～8.0％.
Trimethoprim molecularly imprinted polymer (MIP) was prepared as the coating of stir bar sorptive extraction (SBSE) and applied to the trace analysis of trimethoprim and three sulfonamides in complex samples.The MIP-coating was about 21.5 μm thickness with the relative standard deviations (RSD) of 5.9％ (n=10).It was homogeneous and dense with good thermal and chemical stability.The extraction capability of the MIP-coating was 1.7 times over that of the non imprinted polymer (NIP) coating.The MIP coating exhibited selective adsorption ability to sulfonamides,triazines and methotrexate besides antibacterial synergists.The methods for the determination of trimethoprim and three sulfonamides by MIP-coated stir bar sorptive extraction coupled with HPLC were developed.It was successfully applied to the trace trimethoprim analysis in spiked urine and plasma samples.The linear range was 5 to 200 μg/L and the detection limit was 1.6 μg/L.The recoveries in urine and plasma samples were 84.5％ to 91.7％ with RSDs of 2.9％ -4.4％,71.9％ to 85.1％ with RSDs of 3.0％ -7.3％,respectively.The trimethoprim MIP-coated stir bar was also applied to the trace sulfonamides analysis in spiked milk sample.The linear range was 10-200 μg/L,the detection limit was within the range of 4.5-6.1 μg/L,and the recovery was 83.2％ - 110.2％ with RSDs of 4.1％ -8.0％.
