摘要
目的:建立盐酸尼卡地平中多种有机溶剂残留量的测定方法。方法:采用顶空气相色谱内标法,色谱柱为DB-624毛细管柱(30 m×0.53 mm,3.0μm),载气为氮气,氢火焰离子化检测器,柱温程序升温(初始柱温40℃维持11 min,以40℃·min^(-1)的速率升温至200℃,维持5 min。结果:7种组分甲醇、乙醚、丙酮、异丙醇、乙酸乙酯、三氯甲烷和苯,在此条件下能有效分离,线性范围分别为149.82~898.92μg·m L1(r=0.9997)、264.50~1587.00μg·m L^(-1)(r=0.9994)、252.90~1770.30μg·mL^(-1)(r=0.9979)、250.00~1500.00μg·mL^(-1)(r=0.9997)、251.56~1509.36μg·mL^(-1)(r=0.9997)、6.534~22.869μg·mL^(-1)(r=0.9995)、0.242~0.847μg·mL^(-1)(r=0.9998),平均回收率分别为90.48%(RSD%=3.38%),105.64%(RSD%=3.42%),103.55%(RSD%=3.95%),95.66%(RSD%=3.83%),104.70%(RSD%=2.85%),94.61%(RSD%=3.59%),99.09%(RSD%=6.21%),(n=9),检测限(LOD)分别为:0.15,0.026,0.015,0.25,0.25,3.27,0.12μg·mL^(-1)。结论:该方法简单、准确、灵敏度高、重复性好,适合于盐酸尼卡地平中残留溶剂的检测。
Objective:To establish a headspace gas chromatography method for the determination of residual solvents in decitabine.Methods:A headspace gas chromatography with an internal standard was used with a capillary column DB-624(30 m×0.53 mm,3.0 μm),and with nitrogen as the carrier and an FID as the detector. The column temperature was programmed raising( the initial temperature was 40 ℃,maintaining for 11 min,and rose to 200 ℃ at the rate of 40 ℃ · min^(-1),maintaining for 5 min.Results:The linear range for methanol,methyl formate,acetonitrile and methyl p-toluate was 149.82~898.92 μg·mL^(-1)(r=0.9997)、264.50~1587.00 μg·mL^(-1)(r=0.9994)、252.90~1770.30 μg·m L^(-1)(r=0.9979)、250.00~1500.00 μg·mL^(-1)(r=0.9997)、251.56~1509.36 μg·mL^(-1)(r=0.9997)、6.534~22.869 μg · mL^(-1)(r=0.9995)、0.242~0.847 μg · m L^(-1)(r=0.9998),respectively. The average recovery was 90.48%(RSD% =3.38%),105.64%(RSD%=3.42%),103.55%(RSD%=3.95%),95.66%(RSD%=3.83%),104.70%(RSD%=2.85%),94.61%(RSD%=3.59%),99.09%(RSD%=6.21%),(n=9),and the LOD were 0.15,0.026,0.015,0.25,0.25,3.27,0.12μg · mL^(-1),respectively.Conclusion:The method is simple,accurate,sensitive and reproducible.It can be used for the determination of various residual solvents in decitabine.
作者
高睿
于明
黄海
GAO Rui;YU Ming;HUANG Hai(Liaoning Institute for Drug Control,Shenyang 110036,China)
基金
辽宁省自然基金资助计划(2019-MS-185)。
关键词
盐酸尼卡地平
顶空气相色谱法
残留溶剂
Nicardipine hydrochloride
headspace gas chromatography
residual solvents
