分散固相萃取-气相色谱法测定薰衣草中4个特征成分含量  

Determination of four characteristic components in lavender by dispersive solid phase extraction and gas chromatography

作　　者：孔芳芳 曹建敏[1] 王曙光 庞雪莉[1] 别瑞 孔凡玉[1] 邢丽杰[3] 杨建新 KONG Fang-fang;CAO Jian-min;WANG Shu-guang;PANG Xue-li;BIE Rui;KONG Fan-yu;XING Li-jie;YANG Jian-xin(Tobacco Research Institute of Chinese Academy of Agricultural Sciences,Laboratory of Tobacco and Aromatic Plants Quality and Safety Risk Assessment,Ministry of Agriculture and Rural Affairs,Qingdao 266101,China;Graduate School of Chinese Academy of Agricultural Sciences,Beijing 100081,China;Xinjiang Academy of Agricultural and Reclamation Science,Shihezi 832000,China;Perilla Beauty Biotechnology Co.,Ltd.,Yining 835000,China)

机构地区：[1]中国农业科学院烟草研究所,农业农村部烟草和香薰植物产品质量安全风险评估实验室,青岛266101 [2]中国农业科学院研究生院,北京100081 [3]新疆农垦科学院,石河子832000 [4]伊犁紫苏丽人生物科技有限公司,伊宁835000

出　　处：《药物分析杂志》2022年第5期904-912,共9页Chinese Journal of Pharmaceutical Analysis

基　　金：农业国家、行业标准制定和修订项目(农质标函[2019]77);中国农业科学院科技创新工程项目(ASTIP-TRIC-06);国家农产品质量安全风险评估项目(GJFP2019018)。

摘　　要：目的:建立基于气相色谱同时测定薰衣草中樟脑、芳樟醇、乙酸芳樟酯和乙酸薰衣草酯4个特征成分含量的分析方法。方法:样品经丙酮提取,PSA+C_(18)+GCB混合型分散固相萃取剂净化后,气相色谱-氢火焰离子化检测器进行检测。色谱条件为:使用(5%-苯基)-甲基聚硅氧烷毛细管(DB-5MS,30 m×0.25 mm,0.25μm)色谱柱,高纯氮气为载气,进样量1μL,分流比5∶1,载气流速1.5 mL·min^(-1),进样口温度250℃,柱温箱程序性升温(初始温度50℃,保持2 min,然后以5℃·min^(-1)的速率升温至140℃,再以20℃·min^(-1)的速率升温至300℃),检测器温度250℃。结果:4个成分达到完全分离,无干扰峰出现,专属性好;标准工作曲线线性相关系数均大于0.9997;优化的试验条件下,低、中、高3个添加水平下回收率在89.9%~99.1%;日内和日间RSD在1.0%~2.6%和1.8%~3.7%;方法检测限和定量限在0.818~1.49 mg·kg^(-1)和2.73~4.98 mg·kg^(-1);耐用性试验结果RSD均小于2.3%;5个薰衣草样品中上述4个成分的含量范围分别为2.86~5.53、0.229~2.14、6.03~11.0、0.967~1.38 mg·g^(-1)。结论:建立的方法具有操作简单,重复性好,准确度高等特点,可为薰衣草资源的品质评价和综合利用提供技术支撑,也可为薰衣草特征成分检测标准的制定提供数据支持。Objective:To establish a method for the simultaneously determining the contents of four characteristic components,camphor,linalool,linalyl acetate,and lavandulyl acetate in lavender by gas chromatography.Methods:The samples were extracted with acetone,cleaned up by dispersive solid phase of PSA+C_(18)+GCBand analyzed by gas chromatography with a flame ionization detector(GC-FID).Chromatographic separations were performed in(5%-phenyl)-methylpolysiloxane capillary column(DB-5 MS,30 m×0.25 mm,0.25μm).The oven temperature was programmed from 50℃(2 min),to 140℃at rate 5℃·min^(-1),then to 300℃atrate 20℃·min^(-1).Samples were injected at a 5∶1 split ratio and nitrogen was used as the carrier gas at a flow rate of 1.5 mL·min^(-1).The temperature of injection port and detector was 250℃.Results:The results showed that the four components were separated completely,and there was no interference peak appeared in the blank solvent,the specificity was good.Satisfactory linearity was obtained in a certain concentration range with linear regression coefficients higher than 0.9997.Under the optimized conditions,the recovery was within the range of 89.9%-99.1%at low,medium and high levels.The intra-day and inter-day precisions expressed as RSD were in the range of 1.0%-2.6%and 1.8%-3.7%,respectively.The limit of detection(LOD)and limit of quantification(LOQ)values were 0.818-1.49 mg·kg^(-1)and 2.73-4.98 mg·kg^(-1).RSDs of durability test were all lower than 2.3%.The contents of four components in the five lavender samples were 2.86-5.53,0.229-2.14,6.03-11.0 and 0.967-1.38 mg·g^(-1),respectively.Conclusion:This proposed method has the advantages of simple operation,good repeatability and high accuracy,which can provide technical support for the quality evaluation and comprehensive utilization of lavender resources,and can also provide data support for the establishment of standards for lavender characteristic components detection.

关 键 词：薰衣草 气相色谱法 分散固相萃取 樟脑 芳樟醇 乙酸芳樟酯 乙酸薰衣草酯 

分 类 号：R917[医药卫生—药物分析学]