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    高效液相色谱法测定胶黏剂中树脂酸的含量

    HPLC Determination of Resin Acids in Adhesives

    • 摘要: 样品2.500 g溶解于乙酸乙酯5 mL中,加入甲醇15 mL涡旋0.5 min,再以6 000 r·min-1转速离心10 min,用甲醇冲洗离心管及沉淀,合并上清液和洗涤液,并定容至25 mL。上述所得溶液以Waters XTerra RP18色谱柱为固定相,乙腈-0.4%(体积分数)乙酸溶液(80+20)混合液为流动相进行高效液相色谱分离。脱氢枞酸、枞酸及其同分异构体的检测波长分别为200,216 nm。树脂酸的质量浓度在1.0~100.0 mg·L-1范围内与其峰面积呈线性关系,脱氢枞酸、枞酸及其同分异构体的测定下限(10S/N)分别为3.0,10.0 mg·kg-1。按标准加入法进行回收试验,回收率在91.9%~98.0%之间,相对标准偏差(n=6)在0.26%~2.8%之间。

       

      Abstract: The sample (2.500 g) was dissolved in 5 mL of ethyl acetate, and 15 mL of methanol was added into the solution to whirl for 0.5 min. The mixture was centrifuged at rate of 6 000 r·min-1 for 10 min, and the centrifuge tube and sedimentation were washed by methanol. The supernatant and washing solution were combined and made its volume up to 25 mL. The above solution obtained was separated by HPLC using Waters XTerra RP18 column as the stationary phase and a mixture of acetonitrile-0.4% (φ) acetic acid solution (80+20) as the mobile phase. Detection wavelengths were 200 nm for dehydroabietic acid and 216 nm for abietic acid isomers. Linear relationships between values of peak area and mass concentration of resin acids were obtained in the range of 1.0-100.0 mg·L-1, with lower limits of determination (10S/N) of 3.0 mg·kg-1 for dehydroabietic acid and 10.0 mg·kg-1 for abietic acid isomers. Test for recovery was made by standard addition method, giving results in the range of 91.9%-98.0%, with RSDs (n=6) ranged from 0.26% to 2.8%.

       

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