柱前衍生-高效液相色谱法测定冰乙酸中微量乙酸酐  

Determination of acetic anhydride in glacial acetic acid by HPLC with pre-column derivatization

作　　者：王锦 黄哲 曹婉 周三云 邵静媛 WANG Jin;HUANG Zhe;CAO Wan;ZHOU Sanyun;SHAO Jingyuan(Zhejiang Sundoc Pharmaceutical Science and Tech Co.,Ltd.,Hangzhou 310051,China)

机构地区：[1]浙江圣兆药物科技股份有限公司,杭州310051

出　　处：《化学分析计量》2024年第8期69-73,共5页Chemical Analysis And Meterage

摘　　要：建立柱前衍生-高效液相色谱(HPLC)联合紫外检测分析方法测定冰乙酸中微量乙酸酐的含量。样品采用吗啡啉为柱前衍生剂,色谱柱为Atlantis T3(250 mm×4.6 mm, 5μm),以磷酸水溶液(pH 3.0)-甲醇(体积比为95∶5)为流动相,流量为1.0 mL/min,柱温为30℃,检测波长为210 nm。乙酸酐的质量浓度在2.60~25.97μg/mL范围内与色谱峰面积线性关系良好,相关系数为0.999 9,检出限为0.8μg/mL,定量限为3μg/mL。平均样品加标回收率为92.8%~99.2%,测定结果的相对标准偏差为0.9%~2.3%(n=6)。该方法可用于冰乙酸中微量乙酸酐的含量测定。A pre-column derivatization-high performance liquid chromatography(HPLC)combined with ultraviolet(UV)detection method was established for the determination of trace acetic anhydride in glacial acetic acid.Morpholine was used as the pre-column derivatization agent,and the separation was performed on a Atlantis T3 column(250 mm×4.6 mm,5μm)with phosphoric acid solution(pH 3.0)-methanol(volume ratio was 95∶5)as the mobile phase at 1.0 mL/min.The column temperature was 30℃and the detection wavelength was 210 nm.The mass concentration of acetic anhydride had a good linear relationship in the range of 2.60-25.97μg/mL with the chromatographic peak area,and the correlation coefficient was 0.9999.The limit of detection was 0.8μg/mL,and the limit of quantitation was 3μg/mL.The average recoveries of sample spiking were 92.8%-99.2%,and the relative standard deviations of the determination results were 0.9%-2.3%(n=6).The method is suitable for the quality control of acetic anhydride in glacial acetic acid.

关 键 词：吗啡啉 乙酸酐 冰乙酸 柱前衍生 高效液相色谱法 

分 类 号：O657.7[理学—分析化学]