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气相色谱法测定吡唑硼酸频哪酯及方法学验证

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(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。
GC Determination of Pyrazole Boronic Acid Pinacol Ester and Validation of Analytical Method
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.

GC methodpyrazole boronic acid pinacol estervalidation of analytical method

王武宝、高思国、刘水莲、范荣荣、任耀辉、马雪、张雨

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济南尚博医药股份有限公司,山东 济南 250204

气相色谱法 吡唑硼酸频哪酯 方法学验证

2024

云南化工
云南省化工研究院 云天化集团有限责任公司 云南煤化工集团有限公司 云南省化学化工学会

云南化工

影响因子:0.272
ISSN:1004-275X
年,卷(期):2024.51(1)
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