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基于分析物的分离度和稳定性优化气相色谱-质谱联用条件以同时测定三种姜黄根茎中的九种倍半萜类化合物。

Optimization of GC-MS conditions based on resolution and stability of analytes for simultaneous determination of nine sesquiterpenoids in three species of Curcuma rhizomes.

作者信息

Yang F Q, Li S P, Zhao J, Lao S C, Wang Y T

机构信息

Institute of Chinese Medical Sciences, University of Macau, Taipa, Macau.

出版信息

J Pharm Biomed Anal. 2007 Jan 4;43(1):73-82. doi: 10.1016/j.jpba.2006.06.014. Epub 2006 Jul 24.

Abstract

GC-MS is a powerful tool for analysis of volatile oil, and resolutions of analytes were exclusively used as marker for optimization of the conditions. However, volatile oil usually contains heat labile components which may degrade and result in wrong results during GC analysis. In present study, based on both resolutions and stabilities of 11 sesquiterpenoids, GC-MS conditions were optimized for simultaneously quantitative determination of nine compounds including beta-elemene, curzerene, curcumol, isocurcumenol, germacrone, curdione, curcumenol, neocurdione and curcumenone in Ezhu. However, the other two compounds, i.e. furanodienone and furanodiene, were still thermal sensitive and not available for GC analysis. The results showed that both resolutions and stabilities of analytes should be considered for optimization of GC conditions because the properties of most components in volatile oil are unknown. Under optimum conditions, a capillary column (30 m x 0.25 mm i.d.) coated with 0.25 microm film 5% phenyl methyl siloxane was used for separation. Pulsed splitless inlet with temperature of 190 degrees C was selected for sample injection (0.2 microl). The calibration curves of nine sesquiterpenoids showed good linearity (r2>0.9989) within test ranges. The optimized method showed good repeatability for quantification of these nine components in Ezhu with intra- and inter-day variations of less than 1.42% and 2.79%, respectively. The validated method was successfully applied to quantify 9 sesquiterpenoids in 18 samples of 3 species of Curcuma used as Ezhu.

摘要

气相色谱-质谱联用(GC-MS)是分析挥发油的强大工具,分析物的分离度被专门用作优化条件的指标。然而,挥发油通常含有热不稳定成分,在气相色谱分析过程中可能会降解并导致错误结果。在本研究中,基于11种倍半萜类化合物的分离度和稳定性,对GC-MS条件进行了优化,以同时定量测定莪术中的9种化合物,包括β-榄香烯、莪术烯、莪术醇、异莪术烯醇、吉马酮、莪术二酮、莪术烯醇、新莪术二酮和莪术酮。然而,另外两种化合物,即呋喃二烯酮和呋喃二烯,仍然对热敏感,无法用于气相色谱分析。结果表明,在优化GC条件时应同时考虑分析物的分离度和稳定性,因为挥发油中大多数成分的性质未知。在最佳条件下,使用涂有0.25μm膜厚5%苯基甲基硅氧烷的毛细管柱(30 m×0.25 mm内径)进行分离。选择脉冲不分流进样口,进样温度为190℃,进样量为0.2μL。9种倍半萜类化合物的校准曲线在测试范围内显示出良好的线性(r2>0.9989)。该优化方法对莪术中这9种成分的定量具有良好的重复性,日内和日间变化分别小于1.42%和2.79%。该验证方法成功应用于3种用作莪术的姜黄属植物18个样品中9种倍半萜类化合物的定量分析。

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