HPLC–ELSD法测定三乙醇胺单、双、三酯季铵盐的含量

建立正相高效液相色谱–蒸发光散射检测法测定工业样品中的三乙醇胺单、双、三酯季铵盐的含量。以正己烷–甲醇–四氢呋喃(体积比85∶10∶5,加0.5 mL三氟乙酸调节至pH 3.50)为流动相,等度洗脱三乙醇胺单、双、三酯季铵盐,色谱柱为HP–氨基正相柱,柱温27℃,流量1.0 mL/min,蒸发光散射检测器漂移管温度80℃,载气流量2.6 L/min。三乙醇胺单、双、三季铵盐质量浓度的自然对数与各自对应的色谱峰面积和的自然对数呈良好的线性,相关系数(r~2)分别为0.991 4,0.996 7,0.991 5。测定结果的相对标准偏差为0.6%~2.6%(n=6),加标回收率分别为98.6%,101.2%,97.9%。该方法准确快速,可以为三乙醇胺单、双、三酯季铵盐的生产工艺优化提供理论数据。

Determination of Triethanolamine Monoester,Diester and Triester Ammonium Salt by HPLC-ELSD

A method for the determination of triethanolamine monoester,diester and triester ammonium salt by NP–HPLC–ELSD was established. Mobile phase was hexane–methanol–tetrahydrofuran (85∶10∶5,pH was adjusted to 3.50 by adding 0.05 mL trifluoroacetic acid). Chromatographic column was HP–Amino positive phase column,the column temperature was 27 ℃,the flow rate was 1.0 mL/min,evaporative light-scattering detector drift tube temperature was 80℃,and carrier gas flow rate was 2.6 L/min. Natural logarithm of mass concentration of triethanolamine monoester, diester and triester ammonium salt was linear with the natural logarithm of there chromatographic peak area, the relative coefficient (r2) were 0.991 4, 0.996 7, 0.991 5,repectively. The relative standard deviation of detection results was 0.6%–2.6%(n=6),and addition recoveries were 98.6%,101.2%, 97.9%,respectively. The method is fast and accurate, it can provide theoretical data for the optimization of production technology of triethanolamine monoester,diester and triester ammonium salt.