静态顶空气相色谱法测定标准桃金娘亚微乳中α-蒎烯含量及包封率

Static Headspace Gas Chromatography Standards Act Myrtle Submicroemulsion in α-Pinene Content and Entrap-ment Efficiency

关键词:  顶空气相色谱法  α-蒎烯  标准桃金娘亚微乳  含量测定  包封率

Key words:  headspace gas chromatography  α-pinene  standard myrtle submicroemulsion  content determination  encapsulation efficiency

摘要:

目的 建立静态顶空毛细管气相色谱法测定标准桃金娘亚微乳中α-蒎烯含量及包封率的方法。方法 静态顶空进样条件：顶空加热箱温度设定为90 ℃，定量环温度为100 ℃，传输线温度为110 ℃，GC循环时间为35 min，顶空样品瓶平衡时间为30 min。毛细管气相色谱法：柱温由50 ℃保持1 min，以0.5 ℃·min^-1升温至62 ℃，然后以15 ℃·min^-1升温至180 ℃；FID检测器温度250 ℃，进样口温度230 ℃。乳液稀释样本直接顶空法测定α-蒎烯游离浓度，同量的另一份样本完全破乳后测定α-蒎烯总浓度，根据不同公式及标准曲线分别计算含量及包封率。结果 α-蒎烯浓度在0.001~0.10 μL·mL^-1内线性关系良好，相关系数r=0.999 3。高、中、低浓度加样回收率分别为88.44%，87.39%，105.62%。结论 此方法前处理简单，灵敏度高，选择性好，适合乳液中α-蒎烯的含量及包封率测定。

Abstract:

OBJECTIVE to develop a determinative method analyzing content of α-pinene in standards myrtle submicroemulsion with utilizing the static headspace gas chromatography method. METHODS Static headspace condition: headspace heating oven temperature 90 ℃, loop temperature 100 ℃, the transmission line temperature 110 ℃, GC cycle time of 35 min, headspace vial equilibration time 30 min; GC method: column temperature maintained at 50 ℃ for 1 min, then heated from 0.5 ℃·min^-1 to 62 ℃; afterwards from 15 ℃·min^-1 to 180 ℃; FID detector temperature 250 ℃, inlet temperature 230 ℃. a diluted emulsion samples from direct headspace assay α-pinene free concentration was measured after the total concentration of α-pinene while content and entrapment rate of another equivalent sample, which was completely broken, were calculated according to different formulas and standard curve. RESULTS At the concentration degree of 0.001-0.10 μL·mL^-1, the α-pinene has shown good linear relationship, correlation coefficient r=0.999 3. The samples with high, medium, and low concentration of adding rate were recovered at the ratio of 88.44%, 87.39%, 105.62%, respectively. CONCLUSION This analytical method is featured with simple procedure, high sensitivity, and effective selectivity. It thus can be applied to determine content and entrapment efficiency of α-pinene in the emulsion.