高效液相色谱法测定丙烯酸高碳烷基酯  

Determination of acrylic acid high-carbon ester by high performance liquid chromatography

作　　者：岳娜 马政生[1] 房禹 朱泽波 Yue Na;Ma Zhengsheng;Fang Yu;Zhu Zebo(Chemical Engineering Institute,Northwest University,Xi’an Shaanxi 710069,China)

机构地区：[1]西北大学化工学院,陕西西安710069

出　　处：《石油化工》2018年第11期1247-1252,共6页Petrochemical Technology

摘　　要：建立了一种快速测定丙烯酸高碳烷基酯的反相高效液相色谱法。丙烯酸高碳烷基酯粗产品经深共晶溶剂处理后,静置、分液,得到上层清液即为丙烯酸高碳烷基酯待测试样。利用高效液相色谱采用外标法对试样进行分离、检测,得到最佳色谱条件,并测定了该分析方法的精密度、准确度、定量限及检出限。实验结果表明,最佳色谱条件为采用Syncronis C18色谱柱(250 mm×4.6 mm×5μm)和UV检测器,以V(甲醇)∶V(乙腈)∶V(异丙醇)=70∶25∶5的甲醇-异丙醇-乙腈为流动相,采用等度洗脱的方式,流速1.0 mL/min,检测波长为208 nm,柱温30℃,进样量20μL。该分析方法的加标回收率为94.6%～112.7%、相对标准偏差为0.102%～0.770%、检出限为0.000 15～0.006 27 mg/L、定量限为0.000 5～0.020 9 mg/L;标准曲线线性范围为100～700 mg/L(相关系数大于0.999 0)。该方法快速准确、重现性好,能达到定量检测丙烯酸高碳烷基酯的目的。A rapid analytical method based on reversed-phase high performance liquid chromatography(HPLC)has been established for acrylic acid high-carbon ester.The raw acrylic acid high-carbon esters were treated by deep eutectic solvents,and allowed to stand still and separate,and then the upper clear liquids were purified acrylic acid high-carbon ester samples.The samples were separated and detected by HPLC with the external standard method,and then the optimum chromatography conditions were got.In addition,precision,accuracy,limits of detection and limits of quantification were tested.HPLC separation was carried out on Syncronis C18 column(250 mm×4.6 mm×5μm)and UV detector under the conditions of mobile phase methanol-isopropanol-acetonitrile(volume ratio 70∶25∶5),isocratic elution,flow rate 1.0 mL/min,detection wavelength 208 nm,column temperature 30℃,and injection volume 20μL.The recoveries were 94.6%-112.7%with the relative standard deviations of 0.102%-0.770%,and the limit of detection and the limit of quantification were 0.000 15-0.006 27 mg/L and 0.000 5-0.020 9 mg/L,respectively.A linear standard curve was obtained between 100 and 700 mg/L(correlation coefficient more than 0.999 0).The results showed that the method was rapid,accurate and reproducible,and could achieve the purpose of quantitative detection.

关 键 词：高效液相色谱法 丙烯酸高碳烷基酯 UV检测器 

分 类 号：TQ225.24[化学工程—有机化工]