水中12种醛类化合物的高效液相色谱测定法

Determination of Twelve Kinds of Carbonyl Compounds in Water by High Performance Liquid Chromatography

目的建立水中醛类化合物高效液相色谱(HPLC)测定方法。方法样品经过衍生后,使用C18柱分离,以HPLC-PDA检测12种醛类(甲醛、乙醛、丙醛、丁烯醛、丁醛、戊二醛、戊醛、己醛、庚醛、辛醛、壬醛、癸醛)。以乙腈为流动相A,高纯水为流动相B,梯度淋洗,柱温为30℃,流量为0.8ml/min,检测波长为360nm。结果本方法同时测定12种醛类化合物,在给定浓度范围内各醛类化合物的峰面积与浓度具有良好的线性关系,其中甲醛、乙醛、丙醛、丁醛、戊醛、己醛、丁烯醛、壬醛的线性范围是0.01～5.00μg/ml,庚醛、辛醛、癸醛、戊二醛的线性范围是0.05～5.00μg/ml;检出限的范围是0.005～0.05μg/ml,相关系数>0.9927。添加一定浓度的醛类化合物标准品测定其平均回收率为80.0%～107%,RSD为0.16%～1.69%(n=6)。结论该方法可同时测定12种醛类化合物,分离效果好,抗干扰能力强,方法简便、快捷,回收率高,重现性好,可用于多种醛类化合物的同时检测。

Objective To develop a high performance liquid chromatography （LC） method for simultaneous determination of carbonyl compounds in water. Methods The carbonyl compounds in water were derived with 2,4-DNPH. The derivatives could be separated completely using C_18 column and gradient at holding column temperature （ 30℃） under PDA detector at 360 nm. Mobile phase A was acetonitrile, mobile phase B was water with the flow rate of 0.8 ml/min. Results In the given concentrations, a good linear relation was seen between the concentration of the carbonyl compounds and the peak areas, as for HCHO, CH3CHO, C2H5CHO, C3H5CHO, C4H9CHO, C5H11CHO, C3H5CHO and C8H17CHO, the linear ranges were 0.01-5.00μg/ml, as for C6H13CHO, C7H15CHO, C9H19CHO and C3H7 （CHO）2, the linear ranges were 0.05-5.00μg/ml. The detection limit ranges were 0.005-0.05μg/ml, r〉0.992 7. The recovery rates were 80.0%-107% and the RSDs were between 0.16%-1.69%. Conclusion This method is simple, rapid, sensitive, accurate and is applicable to the simultaneous determination of carbonyl compounds in water.