高衎, 周洁, 李春刚, 唐祁匀. 气相色谱法测定化合物中R-氯甘油的含量[J]. 分析测试技术与仪器, 2019, 25(4): 288-292. DOI: 10.16495/j.1006-3757.2019.04.012
引用本文: 高衎, 周洁, 李春刚, 唐祁匀. 气相色谱法测定化合物中R-氯甘油的含量[J]. 分析测试技术与仪器, 2019, 25(4): 288-292. DOI: 10.16495/j.1006-3757.2019.04.012
GAO Kan, ZHOU Jie, LI Chun-gang, TANG Qi-yun. Detection of (R)-(-)-3-Chloro-1, 2-Propanediol in Compounds by Gas Chromatography[J]. Analysis and Testing Technology and Instruments, 2019, 25(4): 288-292. DOI: 10.16495/j.1006-3757.2019.04.012
Citation: GAO Kan, ZHOU Jie, LI Chun-gang, TANG Qi-yun. Detection of (R)-(-)-3-Chloro-1, 2-Propanediol in Compounds by Gas Chromatography[J]. Analysis and Testing Technology and Instruments, 2019, 25(4): 288-292. DOI: 10.16495/j.1006-3757.2019.04.012

气相色谱法测定化合物中R-氯甘油的含量

Detection of (R)-(-)-3-Chloro-1, 2-Propanediol in Compounds by Gas Chromatography

  • 摘要: 建立了气相色谱法测定化合物中R-氯甘油含量的方法.试验条件:FID检测器,检测器温度为290℃;进样口温度280℃,分流比1:1;载体为氮气,流速5 mL/min;柱温初始温度75℃,保持3 min,以20℃/min的升温速率上升到150℃,再以8℃/min的升温速率上升到180℃,以30℃/min的升温速率上升到240℃,并维持12.5 min.试验结果:空白溶剂不干扰测定,R-氯甘油峰与其他残留溶剂峰分离度良好,检测限为2.06 ng,定量限为6.58 ng,方法专属、灵敏.在80~200 μg/ml范围内,R-氯甘油浓度与峰面积的线性关系良好,线性方程为y=2.558 8x-62.469,线性回归系数r为0.999 4.同一溶液连续进样6次,结果之间的RSD低于1.0%,方法进样精密度良好.同一均质样品平行测定6份,结果之间的RSD低于1.5%,方法重复性良好.加样回收率结果均介于98%~102%之间,方法准确度良好.方法适用于胆碱类物质中R-氯甘油含量的测定.

     

    Abstract: A method to determine (R)-(-)-3-Chloro-1, 2-propanediol in compounds by gas chromatography(GC) is set up. With the FID detector temperature:290℃, inlet temperature:280℃, split ratio 1:1, carrier gas:N2, flow rate:5 mL/min. The column temperature program:initial temperature 75℃ hold for 3 min, heat up to 150℃ at a rate of 20℃/min, and then heat up to 180℃ at a rate of 8℃/min, at last heat up to 240℃ at a rate of 30℃/min and hold for 12.5 min. The blank solution had no interference on the solvents to be tested, (R)-(-)-3-Chloro-1, 2-propanediol peak was well separated from other residual solvent peaks, so the specificity was good. The LOQ was 2.06 ng, the LOD was 6.58 ng, and the linearity was acceptable. The linear relationship between (R)-(-)-3-Chloro-1, 2-propanediol concentration and peak area, in the range of 80~200 μg/mL was good, linear equation:y=2.558 8x-62.469, correlation coefficient r was 0.999 4. The same solution has been injected continuously for 6 times, and the RSD among the results was less than 1.0%.The RSD of the same homogenous sample was less than 1.5%, so the method reproducible. All the results of spiked recovery were in the range of 98%~102%, so the method is accurate. The method is suitable for testing (R)-(-)-3-Chloro-1, 2-propanediol in choline.

     

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