Hariharan M, VanNoord T, Cameron O G, Curtis G C, Ostrow D G
Department of Psychiatry, University of Michigan Medical School, Ann Arbor 48109-0656.
Clin Chem. 1989 Feb;35(2):202-5.
We describe a simple "high-performance" liquid-chromatographic method for determining free 3-methoxy-4-hydroxyphenylglycol (MHPG) in plasma, with coulometric detection and with 4-methoxy-3-hydroxyphenylglycol (iso-MHPG) as the internal standard. MHPG and iso-MHPG are extracted from plasma into ethyl acetate and the extract is washed with a sodium bicarbonate solution, evaporated, reconstituted, and injected into a 25 x 0.4 cm column packed with 3-micron particles of C18 material. We used a mobile phase of acetate buffer (100 mmol/L, pH 5.0) and methanol (92:8 by vol) and an oxidation voltage of 0.5 V. The detection limit of the assay is 0.1 micrograms/L. The interassay CV for a sample with a mean MHPG concentration of 3.84 micrograms/L was 5.2%. The average absolute recovery for the method was 37%.
我们描述了一种简单的“高效”液相色谱法,用于测定血浆中游离的3-甲氧基-4-羟基苯乙二醇(MHPG),采用库仑检测法,并以4-甲氧基-3-羟基苯乙二醇(异-MHPG)作为内标。将MHPG和异-MHPG从血浆中萃取到乙酸乙酯中,萃取液用碳酸氢钠溶液洗涤,蒸发,复溶,然后注入到一根填充有3微米C18材料颗粒的25×0.4厘米色谱柱中。我们使用乙酸盐缓冲液(100 mmol/L,pH 5.0)和甲醇(体积比92:8)作为流动相,氧化电压为0.5 V。该测定法的检测限为0.1微克/升。对于平均MHPG浓度为3.84微克/升的样品,批间变异系数为5.2%。该方法的平均绝对回收率为37%。