摘要
目的:研究十二烷基硫酸钠中脂肪醇组成的测定方法。方法:采用加酸回流的前处理方法将烷基硫酸钠转化为脂肪醇;采用气相色谱直接进样,HP-5(30 m×320μm,0.25μm)、RTX-5(30 m×320μm,0.25μm)毛细管色谱柱;进样口温度为270℃,FID检测器温度为300℃;分流比为10∶1;升温程序:80℃保持5 min,以10℃ min^-1的速率升至180℃,保持6 min,以10℃ min^-1的速率升至280℃,保持5 min。采用面积归一化法计算各脂肪醇组成。结果:在选定的色谱条件下,辛醇、癸醇、十二烷醇、十四醇和十六醇5个组分可达到有效分离;精密度和稳定性的RDS均不大于2.0%,各脂肪醇的检出限均为2μg mL^-1。测定供试品15批,国产和进口十二烷基硫酸钠辅料样品其脂肪醇组成差别显著;分析纯和色谱纯十二烷基硫酸钠试剂其脂肪醇组成差别显著。结论:本方法适用于十二烷基硫酸钠中脂肪醇组成的测定,为十二烷基硫酸钠品种的标准完善、产品的控制和分型提供技术支撑。
Objective:To study the determination method of fatty alcohol composition in sodium lauryl sulfate.Methods:Alkyl sodium sulfate was converted into fatty alcohol by acid reflux pretreatment method.The test was performed by gas chromatography with direct injection.The capillary columns RTX-5(30 m×320μm,0.25μm)and HP-5(30 m×320μm,0.25μm)were used,injection port temperature was 270℃,FID detector temperature was 300℃,and split ratio was 10∶1.The programmed temperature procedure was as follow:keep 80℃for 5 minutes,rise to 180℃ at the rate of 10℃ min^-1,keep 6 minutes,then rise to 280℃ at the rate of 10℃ min^-1 and keep 5 minutes.The contents of fatty alcohols were calculated by area normalization method.Results:The five components of octanol,decanol,dodecanol,tetradecyl alcohol and cetyl alcohol were effectively separated under the proposed chromatographic condition.The RSDs of precision and stability were not more than 2.0%,and the detection limits of all fatty alcohols were same as 2μg mL^-1.The test results of 15 batches of samples showed that the composition of fatty alcohols in domestic and imported sodium lauryl sulfate excipients had the significant differences.The composition of fatty alcohols in analytical and chromatographic reagents of sodium lauryl sulfate had the significant differences.Conclusion:The established method is suitable for the determination of fatty alcohols composition in sodium lauryl sulfate,and provides technical support for the specification improvement,quality control and classification of sodium lauryl sulfate.
作者
田甜
柳艳云
胡敏
TIAN Tian;LIU Yanyun;HU Min(Hubei Institute for Drug Control,Wuhan 430075,China)
出处
《中国药品标准》
CAS
2019年第5期417-422,共6页
Drug Standards of China
基金
国家药典委员会《中华人民共和国药典》药用辅料标准提高任务
关键词
十二烷基硫酸钠
脂肪醇组成
测定
药用辅料
sodium dodecyl sulfate
fatty alcohol composition
determination
excipient
作者简介
第一作者:田甜,主管药师;研究方向:药包材和药用辅料。Tel:027-87705260;15623790697,E-mail:candytt1982@126.com;通讯作者:胡敏,主任药师;研究方向:药包材和药用辅料。Tel:027-87705262,E-mail:604974761@qq.com。
