气相色谱法测定2-乙基丁醛中7个杂质的含量  

Determination of seven impurities in 2-ethylbutanal

作　　者：潘宪伟 陈思芹 于家艳 PAN Xian-wei;CHEN Si-qin;YU Jia-yan(Suzhou Erye Pharmaceutical Co.,Ltd.,Suzhou 215143,China)

机构地区：[1]苏州二叶制药有限公司,苏州215143

出　　处：《药物分析杂志》2022年第5期838-844,共7页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立气相色谱法(GC)测定2-乙基丁醛中乙醛、丁醛、巴豆醛、丁醇、2-乙基丁醇、2-乙基丁酸和三聚乙醛的含量。方法:采用100%二甲基聚硅氧烷为固定液的毛细管柱(DB-1,0.53 mm×30 m,3μm),起始温度为60℃,维持2 min,以5℃·min^(-1)的速率升温至120℃,维持15.5 min,进样口温度为200℃,氢火焰离子化检测器(FID)温度为260℃,载气为氮气,分流比为40∶1,进样体积1μL,外标法定量。结果:乙醛、丁醛、巴豆醛、丁醇、2-乙基丁醇、2-乙基丁酸、三聚乙醛的质量浓度分别在0.1001~0.3004 mg·mL^(-1)(r=0.9991)、0.2005~0.6015 mg·mL^(-1)(r=0.9994)、0.0255~0.0766 mg·mL^(-1)(r=0.9993)、0.1066~0.3017 mg·mL^(-1)(r=0.9993)、0.1002~0.3006 mg·mL^(-1)(r=0.9985)、0.2501~5.0016 mg·mL^(-1)(r=1.000)、0.0808~2.4233 mg·mL^(-1)(r=0.9993)范围内,峰面积与之呈良好线性关系;平均回收率分别为107.4%、106.9%、100.4%、109.1%、101.8%、103.8%、104.1%,RSD分别为1.1%、1.5%、1.2%、1.9%、1.6%、5.2%、0.50%;3批样品中乙醛、丁醛、巴豆醛、丁醇、2-乙基丁醇、2-乙基丁酸和三聚乙醛含量分别在0.02%~0.31%、0.57%~1.0%、0.01%~0.02%、0.24%~0.33%、未检出~0.25%、2.2%~3.9%、0.66%~1.9%范围内。结论:本试验建立的分析方法分离度好,结果准确,可有效分离并测定2-乙基丁醛中7个杂质的含量,为其质量控制提供保障。Objective:To establish a GC method for simultaneous determination of acetaldehyde,butyraldehyde,crotonaldehyde,tert-butanol,2-ethylbutyl alcohol,2-ethylbutyric acid and paraldehyde in 2-ethylbutanal.Methods:GC method was adopted.The determination was performed on capillary column of Aglient DB-1(30 m×0.53 mm,3μm);the column temperature was programmed to start at 60℃,maintained for 2 min,and then rose to 120℃at a rate of 5℃·min^(-1),maintained for 15.5 min;inlet temperature was 200℃;the temperature of the flame ionization detector was 260℃;nitrogen was used as the carrying gas,the split ratio was 40∶1;the injection volume was 1μL,and quantified by external standard method.Results:The acetaldehyde,butyraldehyde,crotonaldehyde,tert-butanol,2-ethylbutyl alcohol,2-ethylbutyric acid and paraldehyde showed good linearity in the ranges of 0.1001-0.3004 mg·mL^(-1)(r=0.9991),0.2005-0.6015 mg·mL^(-1)(r=0.9994),0.0255-0.0766 mg·mL^(-1)(r=0.9993),0.1066-0.3017 mg·mL^(-1)(r=0.9993),0.1002-0.3006 mg·mL^(-1)(r=0.9985),0.2501-5.0016 mg·mL^(-1)(r=1.000)and 0.0808-2.4233 mg·mL^(-1)(r=0.9993),respectively.The average recoveries were 107.4%(RSD=1.1%),106.9%(RSD=1.5%),100.4%(RSD=1.2%),109.1%(RSD=1.9%),101.8%(RSD=1.6%),103.8%(RSD=5.2%)and 104.1%(RSD=0.50%),respectively.The contents of acetaldehyde,butyraldehyde,crotonaldehyde,tert-butanol,2-ethylbutyl alcohol,2-ethylbutyric acid and paraldehyde in 3 batches were 0.02%-0.31%,0.57%-1.0%,0.01%-0.02%,0.24%-0.33%,not detected-0.25%,2.2%-3.9%and 0.66%-1.9%,respectively.Conclusion:With good resolution and accuracy,the method can be reliably and effectively used in the determination of seven impurities in 2-ethylbutanal as well as provides a guarantee for the quality control of 2-ethylbutanal.

关 键 词：乙基丁醛 乙醛 丁醛 巴豆醛 丁醇 乙基丁醇 乙基丁酸 三聚乙醛 气相色谱 含量测定 

分 类 号：R917[医药卫生—药物分析学]