液相色谱

实验中需要利用高效液相色谱来测藻毒素，不知道用哪种色谱柱，请各位达人帮忙。最好列出色谱柱的品牌和型号，在此谢过了！！！！
如果有相关的文献，也欢迎大家帮忙把文献的信息留下来，再次感谢！！！

对国标(GB/T20466—2006)高效液相色谱(HPLC)法检测水中微囊藻毒素-LR(MC-LR)的方法进行了改进,改进如下:C18柱活化前分别用CH2Cl2和CO(CH3)2清洗固相萃取抽吸管路和C18柱填料;样品富集流速取3~5 mL/min;洗脱液(CH3OH)用量取3 mL;洗脱液流速≤1 mL/min。通过对固相萃取(SPE)操作步骤和色谱条件进行改进,可使高效液相色谱法对MC-LR的最低检测限达10 ng/L,固相萃取对不同浓度MC-LR样品的回收率均高于95%,重现性试验标准偏差0.02 ng/L。

建议朋友，参考这资料也许会有帮助！有问题再讨论！


天然水体中痕量微囊藻毒素的高效液相色谱测定方法优化
cuturl('http://www.antpedia.com/?uid-799-action-viewspace-itemid-70173')

[ 本帖最后由 miracle 于 2010-6-27 14:18 编辑 ]

藻毒素有什么性质？

建议朋友看看这个资料，也许对你会有帮助！

荧光衍生化microcystins微囊藻毒素的HPLC分析
cuturl('http://www.quandao.com.cn/applicationshow_231.html')



荧光衍生化microcystins微囊藻毒素的HPLC分析

Medline Abstract

  K Harada, M Oshikata, T Shimada, A Nagata, N Ishikawa, M Suzuki, F Kondo, M

Shimizu, and S Yamada
High-performance liquid chromatographic separation of microcystins derivatized

with a highly fluorescent dienophile.
Nat Toxins, January 1, 1997; 5(5): 201-7.   

Abstract
Order Full text via Infotrieve

Alert Me when Cited
MatchMaker  

  


Faculty of Pharmacy, Meijo University, Nagoya, Japan. kiharada@meijo-u.ac.jp

  Download to Citation Manager
Alert me when this article is cited
PubMed Citation
Related Articles in PubMed
Order Full text via Infotrieve





Microcystins are potent hepatotoxins produced by cyanobacteria, and are also

tumor promoters as well as potent inhibitors of the catalytic subunits of protein

phosphatases 1 and 2A. In order to establish a physicochemical method for

individual detection and determination of trace amounts of microcystins, we

developed a derivatization method for fluorescence (FL) and chemiluminescence

(CL) detection, in which a highly fluorescent dienophile, DMEQ-TAD (4-[2-(6,7-

dimethoxy-4-methyl-3-oxo-3,4-dihydroquinoxalinyl) ethyl]-1,2,4-triazoline-3,5-

dione), was used as the labeling reagent.

DMEQ-TAD reacted smoothly with the conjugated diene of the Adda moiety to give 2

stereoisomers of the adducts. As a result of the extensive experiments, the

following reaction conditions were optimized for the labeling: sample amount, 10

micrograms; reaction solvent, DMF:acetonitrile (1:1); reaction time, 15 minutes;

reaction temperature, 70 degrees C; amount of DMEQ-TAD used relative to that of

microcystin, 80 equivalent.
The resulting 6 adducts from microcystins-LR, -YR, and -RR can be separated from

one another using the following reversed phase HPLC conditions in combination

with a clean-up using ODS column, Cosmosil 5C18-AR (150 x 4.6 I.D. mm);

mobile phase, methanol:0.05M phosphate buffer (pH 3) (1:1);
flow rate, 1.0 ml/min;
detection, FL lambda ex 370 nm, lambda em 440 nm. The detection limits of the

DMEQ-TAD derivatives were estimated to be 100 and 500 pg for LR, and 65 and 2,500

pg for RR using FL and CL detections, respectively; and the detection behavior

was different from that of the Dns-Cys derivatives, which were more sensitive to

CL than FL.

谢谢您的回复。