气相色谱法测定吡唑硼酸频哪酯及方法学验证
GC Determination of Pyrazole Boronic Acid Pinacol Ester and Validation of Analytical Method
王武宝 1高思国 1刘水莲 1范荣荣 1任耀辉 1马雪 1张雨1
作者信息
- 1. 济南尚博医药股份有限公司,山东 济南 250204
- 折叠
摘要
(目的)建立了测定吡唑硼酸频哪酯的气相色谱法方法,并进行了方法学验证.(方法)采用5%苯基-甲基聚硅氧烷色谱柱(30m×ϕ0.25 mm,0.25 μm)检测器:氢离子火焰检测器;载气:氮气;流速:1.0 mL/min;进样器温度:215℃;检测器温度:295℃;分流比:3∶1;进样量:0.1 μL;柱箱温度:初始50℃,维持2 min,按10℃/min升温至 150℃,维持 0 min,按 30℃/min 升温至 260℃,维持 5 min;氢气流速:30 mL/min;空气流速:300 mL/min;氮气流速:25 mL/min.结果 表明,方法的专属性、重复性、线性、中间精密度及溶液稳定性试验结果均符合要求.(结论)本法操作简单,方法准确,可用于吡唑硼酸频哪酯的测定.
Abstract
Objective:The GC method was established for the detection of pyrazole boronic acid pinacol ester and validation of analytical meth-od.Method:The 5％phenyl-methyl polysiloxane(30 m×φ0.25 mm,0.25 μm)column was used;The detector was FID and the carrier gas was nitrogen with a flow rate of 1.0 mL/min;The injection temperature was 215℃;The detection temperature was 295℃;The split ratio was 3:1;The injection volume was 0.1 μL;The initial column temperature was 50℃and maintained for 2 min,the column temperature was raised to 150℃ at the rate of 10℃/min and then maintained for 0 min,the column temperature was raised to 260℃ at the rate of 30℃/min and then maintained for 5 min;The H2 flow rate was 30 mL/min;The air flow rate was 300mL/min;The N2 flow rate was 25 mL/min.Result:The results of specificity,repeatability,linearity,intermediate precision and solution stability all meet the requirements.Conclusion:This method is fast and accurate that can be used for the determination of related substance of pyrazole boronic acid pinacol ester.
关键词
气相色谱法/吡唑硼酸频哪酯/方法学验证Key words
GC method/pyrazole boronic acid pinacol ester/validation of analytical method引用本文复制引用
出版年
2024
国家科技期刊平台
NSTL
维普
万方数据