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目的:建立同时测定荆芥与连翘混合挥发油中β-蒎烯、胡薄荷酮含量的方法,并优化其混合挥发油提取工艺。方法:采用气相色谱法测定β-蒎烯、胡薄荷酮的含量,色谱柱为Hp-5毛细管色谱柱,检测器为氢火焰离子检测器,程序升温,进样量为0.5 μL,分流比为70 ∶ 1,载气为氮气,进样口温度为250 ℃,检测器温度为280 ℃,空气流速为390 mL/min,氢气流速为36 mL/min,尾吹流速为15 mL/min,氮气流速为1 mL/min。采用水蒸气蒸馏法提取混合挥发油,以浸泡时间、提取时间、加水量、连翘粉碎粒度为考察因素,以挥发油提取量、β-蒎烯含量、胡薄荷酮含量及其综合评分为指标,采用正交试验设计法结合信息熵法优化混合挥发油的提取工艺。结果:β-蒎烯、胡薄荷酮检测进样量线性范围分别为1.575~7.875 μg(r=0.999 9)、1.892~9.46 μg(r=0.999 7);定量限分别为0.10、0.25 μg,检测限分别为0.03、0.08 μg;精密度、稳定性、重复性试验的RSD均小于2%(n=6);加样回收率分别为97.77%~100.01%(RSD=0.93%,n=9)、96.47%~99.00%(RSD=0.89%,n=9)。优化的提取工艺为浸泡2 h、提取6 h、加入10倍量水(mL/g)、连翘粒度半瓣。在此条件下,挥发油提取量、β-蒎烯含量、胡薄荷酮含量分别为 3.6 mL、1 450.4 mg、127.6 mg,RSD分别为1.62%、0.20%、1.42%。结论:所建含量测定方法简单、准确,重复性好,优化所得提取工艺稳定、可行。
OBJECTIVE: To establish the method for content determination of volatile oil of Schizonepeta tenuifolia and Forsythia suspensa, and to optimize the extraction technology of the volatile oil. METHODS: The contents of β-pinene and pulegone were determined by GC method. The determination was performed on Hp-5 capillary column. The detector was hydrogen flame ion detector with programmed temperature. The sample size was 0.5 μL, the split ratio was 70 ∶ 1, the carrier gas was nitrogen, the inlet temperature was 250 ℃, the detector temperature was 280 ℃, the air flow rate was 390 mL/min, the hydrogen flow rate was 36 mL/min, the tail flow rate was 15 mL/min, and the nitrogen flow rate was 1 mL/min. Based on single factor test, orthogonal test combined with information entropy method were used to optimize the extraction technology of S. tenuifolia and F. suspensa using soaking time, extraction time, material-liquid ratio and forsythia grain size as factors, with the extraction amount of volatile oil, the content of β-pinene and pulegone and their comprehensive score as indexes. RESULTS: The linear range of β-pinene and pulegone 1.575-7.875(r=0.999 9) and 1.892-9.46 μg(r=0.999 7), respectively. The limits of quantitation were 0.10 and 0.25 μg; the limits of detection were 0.03 and 0.08 μg; RSDs of precision, stability and reproducibility tests were less than 2% (n=6); the recoveries were 97.77%-100.01% (RSD=0.93%,n=9) and 96.47%-99.00%(RSD=0.89%, n=9). The optimal extraction technology was soaking 2 h, extracting for 6 h, 10-fold water (mL/g), half a clove of granularity. Under this condition, the extraction amount of volatile oil, the contents of β-pinene and pulegone were 3.6 mL, 1 450.4 mg, 127.6 mg, respectively. RSD were 1.62%, 0.20%, 1.42%. CONCLUSIONS: Established method is simple, accurate and reproducible, and the optimal extraction technology is stable and feasible.
荆芥连翘混合挥发油水蒸气蒸馏法正交试验信息熵法气相色谱法β-蒎烯胡薄荷酮
Schizonepeta tenuifoliaForsythia suspensaVolatile oilsteam distillationOrthogonal testInformation entropy methodGCβ-pinenepulegone
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