长链烷基甲基萘单磺酸盐和双磺酸盐分离研究

采用反相离子对高效液相色谱(HPLC)及电喷雾质谱(ESI-MS)研究了辛基甲基萘单、双磺酸盐的分离提纯效果.经过大量色谱分析实验,找到了最佳分析条件.紫外检测波长为230nm,流动相为甲醇和水的混合物,流速为0.8mL/min,采用梯度洗脱的方法进行分析.洗脱条件为线性梯度:0~40min,V(甲醇)∶V(水)=60∶40;40~50min,V(甲醇)∶V(水)=100∶0.在此优化条件下样品分离度高,分离效果好.用面积归一化法得到了样品各组分的相对含量,采用HPLC和ESI-MS对组分进行了分析和表征.建立了一种便捷、可靠的烷基甲基萘磺酸盐的分析表征方法以及单、双磺酸盐分离提纯效果的评价方法,得到了满意的结果.

Study of separation of alkylmethylnaphthalene mono- and di-sulfonates

By using high performance liquid chromatography (HPLC) and electrospray mass spectrometry (ESI-MS), the separation effects for octylmethylnaphthalene monosulfonates and octylmethylnaphthalene disulfonates were studied. Through a great deal of analysis tests, the analytical conditions were optimized. Detection was carried out at 230 nm wavelength, different composition mixture of methanol and water were used as eluents, and mobile phase flow velocity is (0.8) mL/min, the linear gradient elution: the volume value of methanol to water is 6040, from 0 min to 40 min; then from 40 min to 50 min, the value is 1000. By using the optimal analytical conditions, the sample compositions were separated in satisfactory result, separation degree was quite high, and analytical time was not too long. Moreover, octylmethylnaphthalene sulfonate surfactants were analyzed and characterized by HPLC and ESI-MS. The characterization method of alkylmethylnaphthalene sulfonates and the evaluation method of separation effect for alkylmethylnaphthalene monosulfonates and alkylmethylnaphthalene disulfonates were established. The satisfactory results were achieved.