岗松油特征图谱的研究及多组分含量测定  

Study on specific chromatogram and determination of chemical components in Baeckea frutescens essential oil

作　　者：白桂昌 罗轶 陆敏仪 

机构地区：[1]广西食品药品检验所,南宁530021

出　　处：《药物分析杂志》2017年第7期1240-1247,共8页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立岗松油的气相特征图谱,研究岗松油的化学成分,建立同时测定岗松油中α-蒎烯、β-蒎烯、α-松油烯、4-异丙基甲苯、桉油精、芳樟醇、4-松油醇、α-松油醇、α-石竹烯、β-石竹烯10种成分含量的气相色谱法。方法:采用GC-MS对岗松油中的共有成分进行鉴定,含量测定采用GC外标法,色谱柱:DB-5气相毛细管色谱柱(柱长60 m,内径0.25 mm,膜厚0.25μm),载气为高纯氮气(99.999%),流速:1.0 mL·min^(-1),分流比10∶1,进样口温度250℃,进样量为1μL,FID检测器,检测器温度250℃,程序升温(初始温度80℃,保持15 min,以每分钟1℃的速率升温至90℃,保持2 min,再以每分钟10℃的速率升温至110℃,每分钟25℃的速率升温至240℃,保持8 min。)结果:岗松油中的14种共有成分得到鉴定,建立了岗松油含12个主要共有峰的气相特征图谱,含量测定中10种主要成分得到良好的分离,在测定范围内的线性关系良好,平均回收率在97%以上。28批岗松油样品10种成分的含量范围:α-蒎烯4.53%~27.51%、β-蒎烯1.10%~14.12%、α-松油烯0.00%~3.69%、4-异丙基甲苯4.65%~17.55%、桉油精6.91%~30.02%、芳樟醇2.75%~9.79%、4-松油醇0.81%~11.19%、α-松油醇0.64%~4.44%、α-石竹烯0.29%~5.93%、β-石竹烯0.18%~7.73%。结论:特征图谱结合多组分的含量测定,能更好地控制岗松油的质量。Objective： To establish GC specific chromatograms of Baeckea frutescens essential oil and to develop a GC method for simultaneous determination of α -pinene, β -pinene, α-terpinene, 4-isopropyltoluene, eucalyptol, linalool, 4-terpineol, α-terponeol, α -caryophyllene, β -earyophyllene in Baeckea frutescens. Methods： GC-MS was applied for the identification of multiple components in Baeckea frutescens. GC was performed on a DB-5 column （ length 60 m, diameter 0.25 ram, thickness of 0.25 μm ）. The carrier gas was high purity nitrogen at a flow rate of 1.0 mL ·min^-1. The inlet temperature was 250 ℃. The injection volume was 1 μL and the FID detector temperature was 250 ℃. The column temperature was increased with following sequence ：initial temperature was 80 ℃, raised to 90 % with a rate of 1 ℃ · min^-1, maintained for 2 min, then raised to 110 ℃ with a rate of 10 ℃· min^-1, raised to 240 ℃ with a rate of 25 ℃ · min^-1, maintained for 8 min. The content ranges of the 10 components of the 28 batch of samples are listed here： α-pinene 4.53%-27.51%, 13-pinene 1.10%- 14.12%, α-terpinene 0.00%-3.69%, 4-isopropyltoluene 4.65%-17.55%, eucalyptol 6.91%-30.02%, linalool 2.75%-9.79%, 4-terpineol 0.81%-11.19%, α-terponeol 0.64%-4.44%, ct-caryophyllene 0.29%-5.93%, β -caryophyllene 0.18%-7.73%. Results： 14 common components were identified by GC-MS in Baeckea frutescens essential oil. The GC specific chromatogram of Baeckea frutescens essential oil with 12 common characteristic peaks was estabhshed. Ten main components were well separated and showed good hnearity in the concentration range of detection, the added sample recovery rate was above 97%. Conclusions： The combination of specific chromatograms and GC determination is capable of effectively controlling the quality of Baeckea frutescens essential oil.

关 键 词：岗松油 特征图谱 气相色谱-质谱联用 Α-蒎烯 Β-蒎烯 α-松油烯 4-异丙基甲苯 桉油 

分 类 号：R917[医药卫生—药物分析学]