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目的:建立离子色谱法同时测定羟苯乙酯中氯离子和硫酸根离子的含量,评价不同级别羟苯乙酯中氯离子和硫酸根离子含量的质量状况。方法:采用色谱柱为Dionex Ion Pac AS_(18)(250 mm×4 mm,5μm),流动相为氢氧化钾淋洗液(梯度洗脱),流速为1.0 ml·min~(-1),进样量为25μl。结果:氯离子和硫酸根离子分别在0.02~4.00μg·ml~(-1)、0.10~10.00μg·ml~(-1)范围内线性关系良好(r分别为0.999 9和0.999 5),氯离子和硫酸根离子回收率分别为90.12%、85.54%,RSD分别为6.2%、3.4%(n=9)。63批样品中,氯离子和硫酸根离子含量分别为0.000 3%~0.015 7%、0.000 9%~0.024 4%。结论:该方法操作简便、快速,结果准确,可用于同时测定羟苯乙酯中氯离子和硫酸根离子的含量,为其质量控制提供保证。
Objective: To establish a method for the simultaneous determination of chloride ion and sulfate ion in phenethyl ethyl ester by ion chromatography, and to evaluate the quality of chloride ion and sulfate ion ion in different levels of ethyl phenethyl ester. Methods: The chromatographic column was Dionex Ion Pac AS_ (18) (250 mm × 4 mm, 5 μm). The mobile phase consisted of potassium hydroxide eluant (gradient elution) at a flow rate of 1.0 ml · min -1. Injection volume of 25μl. Results: The results showed that there was a good linear relationship between chloride ion and sulfate ion in the range of 0.02-4.00 μg · ml -1 and 0.10-10.00 μg · ml -1 (r = 0.999 9 and 0.999 5, respectively), chlorine The ion and sulfate ion recoveries were 90.12% and 85.54%, respectively, with RSDs of 6.2% and 3.4%, respectively (n = 9). The contents of chloride and sulfate in the 63 batches of samples were 0.000 3% to 0.015 7% and 0.000 9% to 0.024 4%, respectively. Conclusion: The method is simple, rapid and accurate. It can be used for the simultaneous determination of chloride ion and sulfate ion in hydroxyphenylacetate to provide assurance for its quality control.