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目的:建立同时测定不同产地荜澄茄挥发油中α-蒎烯、β-蒎烯、月桂烯、柠檬烯、6-甲基-5-庚烯-2-酮和柠檬醛6种成分含量的气相色谱法。方法:采用水蒸气蒸馏法进行挥发油的提取,采用毛细管气相色谱法对挥发油中6种成分进行含量测定。气相色谱条件:DB-17石英毛细管色谱柱(30m×0.25mm×0.25μm);氢火焰离子检测器(FID);进样口温度为230℃;检测器温度为250℃;升温程序为起始温度50℃,以2℃·min-1升至80℃,再以10℃·min-1升至240℃,保持10min;载气为氮气,流速为1.2mL·min-1;进样方式为分流进样,分流比为10∶1;进样量为1μL。结果:α-蒎烯、β-蒎烯、月桂烯、柠檬烯、6-甲基-5-庚烯-2-酮和柠檬醛的线性范围分别为0.0183～0.91mg·mL-1(r=0.9999),0.0099～0.496mg·mL-1(r=0.9999),0.0096～0.478mg·mL-1(r=0.9999),0.101～5.06mg·mL-1(r=1.0),0.095～4.73mg·mL-1(r=0.9999)和0.146～7.35mg·mL-1(r=0.9999);平均回收率(n=9)分别为96.8%～101.2%(RSD=3.1%),96.1%～102.6%(RSD=3.2%),97.6%～103.0%(RSD=3.3%),99.9%～100.9%(RSD=1.4%),98.9%～99.6%(RSD=1.7%)和96.6%～99.7%(RSD=2.6%)。结论:本方法简单、准确、可靠,可作为该药材质量控制的指标。
OBJECTIVE: To establish a gas chromatograph for the simultaneous determination of 6 constituents of α-pinene, β-pinene, myrcene, limonene, 6-methyl-5-hepten-2-one and citral in the volatile oil law. Methods: Volatile oil was extracted by steam distillation. The contents of six components in volatile oil were determined by capillary gas chromatography. Gas chromatographic conditions: DB-17 quartz capillary column (30m × 0.25mm × 0.25μm); hydrogen flame ionization detector (FID); inlet temperature was 230 ℃; detector temperature was 250 ℃; temperature program was started The temperature was raised to 50 ℃, the temperature was raised to 80 ℃ at 2 ℃ · min-1, then the temperature was increased to 240 ℃ at 10 ℃ · min-1 for 10min. The carrier gas was nitrogen and the flow rate was 1.2mL · min-1. Split injection, split ratio of 10: 1 injection volume of 1μL. Results: The linear ranges of α-pinene, β-pinene, myrcene, limonene, 6-methyl-5-hepten-2-one and citral were 0.0183-0.91 mg · mL -1 (R = 0.9999), 0.0096-0.478 mg · mL-1 (r = 0.9999), 0.101-5.06 mg · mL -1 (r = 1.0), and 0.095-4.73 mg · mL (N = 9) were 96.8% ~ 101.2% (RSD = 3.1%), 96.1% ~ 102.6% (r = 0.9999) and 0.146 ~ 7.35 mg · mL- (RSD = 1.3%), 99.9% -100.9% (RSD = 1.4%), 98.9% -99.6% (RSD = 1.7%) and 96.6% -99.7% (RSD = 2.6%). Conclusion: The method is simple, accurate and reliable and can be used as an indicator of the quality control of the medicinal materials.