基于声表面波-气相色谱联用技术快速分析麝香中的麝香酮

Rapid analysis of musk ketone in musk based on gas chromatography-surface acoustic wave technology

建立声表面波气相色谱仪现场快速检测麝香中主要成分麝香酮的方法。取麝香样品经过超声、过滤后,使用声表面波气相色谱仪进行检测。DB-5毛细管色谱柱初始温度45◦C,以10◦C/s程序升温至180◦C,检测器温度40◦C。麝香酮在7 s内出峰,最低检测限为15.8 pg,精密度相对标准偏差值为2.10%3.84%,重复性相对标准偏差值为4.23%,稳定性相对标准偏差值为4.49%,麝香酮溶液在0.210g/mL质量浓度范围内线性良好。测试16组麝香样品,麝香酮含量在2.08%3.83%范围内。麝香酮含量最高的为四川圭兴林麝,含量最低的为陕西凤县林麝。三年生的林麝和马麝中麝香酮含量均大于一年生的林麝和马麝。声表面波气相色谱仪检测麝香酮具有较好的响应特性、精密度、重复性和稳定性,建立的声表面波气相色谱方法能够实现麝香中主要成分麝香酮快速、准确的定量检测。

A rapid detection method of musk ketone which the main component of musk has been developed using gas chromatography with surface acoustic wave detector(GC-SAW).Musk samples were detected by using GC-SAW after ultrasonic and filtration.The initial temperature of DB-5 capillary column was 45◦C,and was temperature-programmed to 180◦C with the rate of 10◦C/s,the detector temperature was 40◦C.The retention time of muscone was in 7 s,the lowest detection quantity was 15.8 pg,the precision relative standard deviation(RSD)value was 2.10%–3.84%,the repeatability RSD value was 4.23%,the stability RSD value was 4.49%.The linearity is good in the concentration range of 0.2–10g/mL.Test 16 groups of musk samples,the content of muscone is between 2.08%and 3.83%.The highest content of musk ketone is the forest musk deer in Guixing,Sichuan,and the lowest content is the forest musk deer in Fengxian,Shaanxi.The content of muscone in three-year-old forest musk deer and horse musk deer is greater than that in one-year-old musk deer.The surface acoustic wave gas chromatograph has good response characteristics,precision and stability for detecting muscone.The established GC-SAW method can realize the rapid and accurate quantitative detection of the main component muscone in musk.