HAOHAN工业用羟丙基甲基纤维素中甲氧基和羟丙氧基含量测定毛细管柱HH-5

本标准规定了工业用羟丙基甲基纤维素型号、要求、试验方法、检验规则、包装、标识、贮存和运输。
本标准适用于以精制棉或其他纤维素为原料，经碱化和醚化生产的工业用羟丙基甲基纤维素。

浩瀚色谱（山东）应用技术开发有限公司建立顶空气相色谱-质谱法(gas chromatography-mass spectrometry,GC-MS)测定低取代羟丙纤维素中羟丙氧基的含量。方法样品在顶空瓶中与氢碘酸反应,使羟丙氧基转为2-碘丙烷,反应结束后加碱液中和过量的氢碘酸防止腐蚀进样器和色谱柱,随后顶空进样,以HH-5毛细管柱分离,GC-MS选择离子检测模式测定。结果羟丙氧基的浓度在0.6435～17.26025 mg/mL的范围内线性关系良好,相关系数r0.999;此方法的检出限(S/N=3)为0.039μg/mL,定量限(S/N=10)为0.13μg/mL;在不同添加水平下,方法的平均回收率为99.4%,相对标准偏差为1.3%(n=3)。结论该方法简便、快速、灵敏、准确,适合羟丙氧基定性和定量测定。
 

名称：毛细管柱
固定相：5%苯基-95%甲基聚硅氧烷
规格：30m*0.32mm*0.25

型号：HH-5

 
This standard specifies the type, requirements, test methods, inspection rules, packaging, labeling, storage and transportation of hydroxypropyl methylcellulose for industrial use.
This standard applies to industrial hydroxypropyl methyl cellulose produced by alkalization and etherification with refined cotton or other cellulose as raw materials.

Haohan Chromatography (Shandong) Application Technology Development Co., Ltd. established a headspace gas chromatography-mass spectrometry (GC-MS) method to determine the content of hydroxypropoxy groups in low-substituted hydroxypropyl cellulose. Method The sample was reacted with hydriodic acid in a headspace vial to convert the hydroxypropoxy group into 2-iodopropane. After the reaction was completed, lye was added to neutralize the excess hydriodic acid to prevent corrosion of the injector and chromatographic column. The samples were injected, separated by HH-5 capillary column, and determined by GC-MS in selected ion detection mode. Results The concentration of hydroxypropoxy was in the range of 0.6435～17.26025 mg/mL with a good linear relationship, and the correlation coefficient was r0.999; the detection limit (S/N=3) of this method was 0.039 μg/mL, and the quantification limit (S /N=10) was 0.13 μg/mL; the average recovery was 99.4% with a relative standard deviation of 1.3% (n=3) at different levels of addition. Conclusion The method is simple, rapid, sensitive and accurate, suitable for the qualitative and quantitative determination of hydroxypropoxy.

Name: capillary column
Stationary Phase: 5% Phenyl-95% Methylpolysiloxane
Specifications: 30m*0.32mm*0.25

Model: HH-5