摘要
提出了固相萃取-高效液相色谱法测定水中微囊藻毒素的方法。水样经减压过滤后,过C18反相固相萃取柱富集浓缩,用20%(体积分数)甲醇溶液淋洗,以1mL.min-1的流速,用纯甲醇将微囊藻毒素从固相萃取柱上洗脱下来,氮吹浓缩后,用0.05mol.L-1磷酸盐缓冲液作流动相,与甲醇以体积比为40比60进行淋洗,紫外检测波长为238nm,用此方法对两种微囊藻毒素MC-LR、MC-RR的线性范围为0.25～10.0mg.L-1,测定限(10S/N)均为0.05μg.L-1,回收率在76.2%～96.5%之间。
A method of determination of microeystin in surface water by HPLC with solid phase extraction （SPE） was proposed. The water sample was first filtered under reduced pressure and microcystin in the filtrate was then enriched by passing through a C18-reversed-phase SPE column, which was eluted with a mixed solution of CH3 OH＋ H2O （mixed in the ratio of 20 ＋ 80 by volume）, to remove substances coexisting with microeystin. The SPE column was dried by blowing with N2-gas, and microcystin was eluted from the column with pure CH3OH at a flow-rate of 1 mL · min^-1. The eluate was collected and evaporated to I mL and used for HPLC determination. The Cosmosil C18 chromatographic column was used as the stationary phase and a mixed solution of 0. 05 mol · L^-1 phosphate buffer solution and methanol, mixed in the ratio of 40 to 60 by volume, was used as mobile phase. UVdetection at 238 nm was adopted in the determination. Under these conditions, 2 isomers of microcystin, i. e , MC-LR and MC-RR, were well separated, and linear relationship between values of peak area and concentration of the 2 isomers was obtained in the range of 0. 25-10. 0 mg · L^-1 , with determination limit （10S/N） of 0. 05 μg · L^-1. Values of recovery found by adding mixed standard solution of the 2 isomers to a blank water sample, were in the range of 76. 2%-96. 5%.
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2008年第12期1176-1178,1181,共4页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
