建立一种快速、准确测定生物样品中左旋多巴(L-DOPA)、去甲肾上腺素(NE)、肾上腺素(E)、多巴柯(DOPAC)、多巴胺(DA)、5-羟吲哚乙酸(5-HIAA)、高香草酸(HVA)及5-羟色胺(5-HT)8种递质含量的高效液相色谱.电化学检测方法。使8种物质在25rain于单一流动相、单流速、单通道检测器情况下达到良好的分离效果。采用ESAMD-150色谱拄(150mm×3.2mm,3μm),流动相为50mmol/L柠檬酸、50mmol/L无水乙酸钠、0.5mmol/L1.庚烷磺酸钠、0.5mmol/L乙二胺四乙酸二钠、5mmol/L三乙胺,pH3.5,在甲醇浓度为5%~10%,流速0.3~0.5mL/min,柱温为30℃时,都能使8种物质很好分离,其中在甲醇浓度8%,流速0.4mL/min,检测到前5种物质线性范围为0.005~10nmol/L;后3种0.001~10nmol/L,8种物质相关系数往0.994~0.999之间,检出限在pmol/L水平;回收率在80.3%~102.1%之间,相对偏差在1.4%~4.8%之侧。且对样本处理和保存方法进行了探讨。
A simple, rapid and sensitive HPLC-ECD method was established to detect the monoamine neuro- transmitters and its metabolites, eight neurotransmitters including L-Dihydroxyphenylalanine(L-DOPA) , Norepinephrine( NE ) ; Eoubeogrube ( e ) ; 3,4-Hydroxyphenylacitie acid ( DOPAC ) ; 3-Hydroxytyramine hydro- chloride ( DA ) ; 5-Hydroxy-3-indoleacetic acid ( 5-HIAA ) ; 4-Hydroxy-3-methoxyacetie acid ( HVA ) ; 5-Hydroxytryamine(5-HT) can be separated and detected under the same mobile phase, flow rate and mono-channel detector in 25 rain. The analytes were separated on a ESA MD-150 column (150 mm× 3.2 ram, 3μm). The mobile phase( pH 3.5 ), consisted of methanol-water phase (containing 50 mmol/L citric acid, 50 mmol/L anhydrous sodium acetate, 0. 5 mmol/L 1-octanesulfonie acid sodium salt, 0. 5 mmol/L Na2EDTA, 5 mmol/L Triethylamine, 5% -10% methanol)the column temperature was kept at 30 ℃. The eight transmitters can be separated at a flow rate of 0.3 -0.5 mL/min using 8% methanol with a flow rate of 0.4 mL/min. The first five components were observed be linear over a concentration range of 0. 005 - 10 nmol/L, and the followed three components 0. 001 - 10 nmol/L. The low limit of detection was the level of pmol/L. The correlation coefficients of these compounds were 0.994-0.999, the recoveries were 80.3% -102.1% , the RSDs were 1.42% -4.85%. The pretreatment of samples was also studied.