高效液相色谱-二极管阵列检测法测定马来酸和乙醛酸

建立了高效液相色谱-二极管阵列法同时测定乙醛酸和马来酸的高效液相色谱方法。色谱条件为:Shim-pack VP.ODS柱(250 mm×4.6 mm I.D.,5μm);二极管阵列检测器;流动相为甲醇/磷酸盐缓冲溶液(NaH2PO4浓度为0.1 mol/L,H3PO4调节至pH=2.98),体积比为5∶95,流速为1.0 mL/min,检测波长为195 nm,柱温为40℃。线性范围分别为79.6～26 660 mg/L和9.3～7 864 mg/L,检出限分别为39.4 mg/L和4.7 mg/L;日内、日间测定的相对标准偏差(RSD):乙醛酸为0.22%和0.46%,马来酸为0.02%和0.03%。

Determination of glyoxylic acid and maleate by high performance liquid chromatography with photodiode array detectors

A precolumn-derivatization method was applied to determine glyoxylic acid and maleate in high performance liquid chromatography(HPLC) was established.The HPLC with photodiode array detection(PAD) was performed on a Shim-pack VP.ODS column(250 mm×4.6 mm I.D.,5 μm).The mobile phase was CH3OH-0.1 mol/L NaH2PO4 buffer solution 5∶95(v/v),of which NaH2PO4 buffer solution was adjusted to pH 2.98 using H3PO4.The flow rate was 1.0 mL/min at the column temperature of 40 ℃ and the detection wave length was 195 nm.The linear range of glyoxylic acid was 79.6~26 660 mg/L while that of maleate was 9.3~7 864 mg/L.The detection limit of glyoxylic acid and maleate was 39.4 mg/L and 4.7 mg/L,respectively.The relative standard deviations(RSD) of inter and intra-day precision experiments were 0.22%,0.46% and 0.02%,0.03%.