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目的建立顶空气相色谱-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HP-5MS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r>0.999;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。
Objective To establish a gas chromatography-mass spectrometry (GC-MS) method for the determination of hydroxypropoxyl in low substituted hydroxypropylcellulose. Method The sample was reacted with hydroiodic acid in a headspace vial to convert the hydroxypropoxyl to 2-iodopropane. After the reaction was over, neutralization with an excess of hydroiodic acid prevented corrosion of the injector and column, followed by headspace The injection was separated on a HP-5MS capillary column and determined by GC-MS selective ion detection mode. Results The linearity of hydroxypropyloxy was in the range of 0.6435-17.26025 mg / mL with the correlation coefficient r> 0.999. The detection limit (S / N = 3) was 0.039 μg / mL and the limit of quantification / N = 10) was 0.13μg / mL. The average recovery of the method was 99.4% at different added levels with a relative standard deviation of 1.3% (n = 3). Conclusion The method is simple, rapid, sensitive and accurate, suitable for qualitative and quantitative determination of hydroxypropoxyl.