环境科学与技术
環境科學與技術
배경과학여기술
ENVIRONMENTAL SCIENCE & TECHNOLOGY
2010年
1期
19-22
,共4页
余婷%谢平%戴明%梁高道
餘婷%謝平%戴明%樑高道
여정%사평%대명%량고도
微囊藻毒素%提取%制备%高效液相色谱-质谱检测
微囊藻毒素%提取%製備%高效液相色譜-質譜檢測
미낭조독소%제취%제비%고효액상색보-질보검측
Microcystins%extraction%preparation%high performance liquid chromatography-mass spectrometry
微囊藻毒素是一类由蓝藻产生的具有肝毒性的生物毒素.微囊藻毒素标准品是开展为微囊藻毒素相关研究的必需的实验材料,文章以滇池天然水华蓝藻为原料,建立了以5%乙酸和75%的甲醇溶液提取,通过优化提取、分离和制备条件,制备了一定量的微囊藻毒素高纯度样品,经HPLC鉴定分析,纯度可达90%以上.文章在相同的质谱条件下分别对MC-LR和[Dha7]MC-LR等毒素进行了质谱检测,一级质谱结果表明,MC-LR和[Dha7]MC-LR的一价电离离子峰分别为995和981,MC-RR的二价电离离子峰为520,并分析它们的二级质谱裂解特征,确定三种毒素化学结构MC-RR为环(Ala-Arg-MeAsp-Arg-Adda-Glu-Mdha)、MC-LR为环(Ala-Leu-MeAsp-Arg-Adda-Glu-Mdha)、[Dha7]MC-LR为环(Ala-Leu-MeAsp-Arg-Adda-Glu-Dha).改良后的检测方法同样应用于检测受微囊藻毒素污染的武汉东湖水样.
微囊藻毒素是一類由藍藻產生的具有肝毒性的生物毒素.微囊藻毒素標準品是開展為微囊藻毒素相關研究的必需的實驗材料,文章以滇池天然水華藍藻為原料,建立瞭以5%乙痠和75%的甲醇溶液提取,通過優化提取、分離和製備條件,製備瞭一定量的微囊藻毒素高純度樣品,經HPLC鑒定分析,純度可達90%以上.文章在相同的質譜條件下分彆對MC-LR和[Dha7]MC-LR等毒素進行瞭質譜檢測,一級質譜結果錶明,MC-LR和[Dha7]MC-LR的一價電離離子峰分彆為995和981,MC-RR的二價電離離子峰為520,併分析它們的二級質譜裂解特徵,確定三種毒素化學結構MC-RR為環(Ala-Arg-MeAsp-Arg-Adda-Glu-Mdha)、MC-LR為環(Ala-Leu-MeAsp-Arg-Adda-Glu-Mdha)、[Dha7]MC-LR為環(Ala-Leu-MeAsp-Arg-Adda-Glu-Dha).改良後的檢測方法同樣應用于檢測受微囊藻毒素汙染的武漢東湖水樣.
미낭조독소시일류유람조산생적구유간독성적생물독소.미낭조독소표준품시개전위미낭조독소상관연구적필수적실험재료,문장이전지천연수화람조위원료,건립료이5%을산화75%적갑순용액제취,통과우화제취、분리화제비조건,제비료일정량적미낭조독소고순도양품,경HPLC감정분석,순도가체90%이상.문장재상동적질보조건하분별대MC-LR화[Dha7]MC-LR등독소진행료질보검측,일급질보결과표명,MC-LR화[Dha7]MC-LR적일개전리리자봉분별위995화981,MC-RR적이개전리리자봉위520,병분석타문적이급질보렬해특정,학정삼충독소화학결구MC-RR위배(Ala-Arg-MeAsp-Arg-Adda-Glu-Mdha)、MC-LR위배(Ala-Leu-MeAsp-Arg-Adda-Glu-Mdha)、[Dha7]MC-LR위배(Ala-Leu-MeAsp-Arg-Adda-Glu-Dha).개량후적검측방법동양응용우검측수미낭조독소오염적무한동호수양.
Microcystins are a kind of hepatotoxic cyanotoxin. Extraction of intracellular Microcystin variants is required to characterize and quantify all microcystins present in a sample. The method was established to isolate and purify Microcystins from natural cyanobacterial bloom dominated by Microcystis aeruginosa in Dianchi Lake, Yunnan Province, by the main steps of extraction with 75% aqueous methanol, 5% acetic acid solution through semi-prep-LC and ODS column with purity over 90%. The study was to develop an appropriate analytical procedure, based on solid phase extraction and liquid chromatography electrospray mass spectrometry for the determination of trace amounts of MCs in water samples. The developed method was applied to analyze the Microcystin-polluted surface water sampled from East Lake, Wuhan.