气相色谱-一测多评法同时测定佛手挥发油中6种成分的含量-中国药房

气相色谱-一测多评法同时测定佛手挥发油中6种成分的含量

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篇名：	气相色谱-一测多评法同时测定佛手挥发油中6种成分的含量
TITLE：	Simultaneous Determination of 6 Components in Volatile Oil from Citrus medica by GC-QAMS
摘要：	目的：建立同时测定佛手挥发油中α-蒎烯、β-蒎烯、月桂烯、柠檬烯、γ-松油烯、α-松油醇等6种成分含量的方法。方法：采用气相色谱-一测多评法。色谱柱为AgilentDB-17毛细管柱，检测器为火焰离子化检测器，载气为氮气（纯度99.999％），载气流速为0.5mL/min，氮气（尾吹）流速为25mL/min，氢气流速为30mL/min，空气流速为400mL/min，进样口温度为250℃，检测器温度为280℃，程序升温，进样量为0.5μL，分流比为35∶1。以柠檬烯为内参物，计算α-蒎烯、β-蒎烯、月桂烯、γ-松油烯等4种成分的相对校正因子，再根据相对校正因子计算佛手挥发油中4种成分的含量，并与内标法（以十二烷为内标物，测定6种成分）进行比较。结果：α-蒎烯、β-蒎烯、月桂烯、柠檬烯、γ-松油烯、α-松油醇检测质量浓度的线性范围分别为0.0305～0.2138、0.0666～0.4660、0.0218～0.1523、0.7652～5.3564、0.3873～2.7108、0.0342～0.2396mg/mL（r均大于0.999）；检测限分别为4.82、7.89、4.01、4.54、5.53、2.47µg/mL，定量限分别为15.34、25.91、13.69、15.70、18.68、8.36µg/mL；精密度、重复性、稳定性（24h）试验的RSD均小于2％；平均加样回收率分别为96.08％、97.48％、100.90％、101.22％、100.54％、95.84％（RSD均小于3％，n＝6）。α-蒎烯、β-蒎烯、月桂烯、γ-松油烯的平均相对校正因子分别为0.9978、1.5307、0.9524、1.0255（RSD均小于1％）。内标法测得α-蒎烯、β-蒎烯、月桂烯、柠檬烯、γ-松油烯、α-松油醇的含量分别为3.2969～20.9941、11.3006～39.4409、3.6842～11.2914、174.8578～511.6118、0～285.1273、0～48.8586mg/g；一测多评法测α-蒎烯、β-蒎烯、月桂烯、γ-松油烯的含量分别为3.2968～20.9940、11.3003～39.4397、3.6841～11.2911、0～285.1266mg/g；两种方法测得α-蒎烯等4种成分含量的相对误差均小于1％。结论：所建气相色谱-一测多评法简便、快捷，准确度高，重复性好，可用于佛手挥发油成分的定量分析及质量控制。
ABSTRACT：	OBJECTIVE：To establish a metho d for simultaneous determinat ion of α-pinene，β-pinene，myrcene，limonene， γ-terpinene and α-terpineol in volatile oil from Citrus medica . METHODS ：GC-QAMS method was adopted. The determination was performed on Agilent DB- 17 capillary column. Flame ionization detector was adopted with nitrogen as carrier gas （purity 99.999％） at the flow rate of 0.5 mL/min. The flow rate of nitrogen （make-up gas ）was 25 mL/min，the flow rate of hydrogen was 30 mL/min， and the flow rate of air was 400 mL/min. The inlet temperature was 250 ℃，and the detector temperature was 280 ℃（programmed temperature），and injection volume was 0.5 μL with split ratio of 35 ∶ 1. Using limonene as internal reference ，relative correction factors of α-pinene，β-pinene，myrcene and γ-terpinene were calculated. The contents of 4 components in the samples were calculated according to the relative correction factors. The results were compared between QAMS and internal standard method （ISM，using dodecane as internal substance ，6 components to be determined ）. RESULTS ：The linear range of α-pinene，β-pinene， myrcene，limonene，γ-terpinene and α-terpineol were 0.030 5-0.213 8，0.066 6-0.466 0，0.021 8-0.152 3，0.765 2-5.356 4，0.387 3- 2.710 8，0.034 2-0.239 6 mg/mL（all r＞0.999）. The limits of detection were 4.82，7.89，4.01，4.54，5.53，2.47 µg/mL，and the limits of quantification were 15.34，25.91，13.69，15.70，18.68，8.36 µg/mL，respectively. RSDs of precision ，repeatability and stability tests （24 h）were all less than 2％. The average recovery rates were 96.08％，97.48％，100.90％，101.22％，100.54％， 95.84％（all RSD ＜3％，n＝6）. The average relative correction factors of α-pinene，β-pinene，myrcene and γ-terpinene were 0.997 8， 1.530 7，0.952 4 and 1.025 5 （all RSD ＜1％）. The contents of α-pinene，β-pinene，myrcene，limonene，γ-terpinene and α-terpineol by ISM were 3.296 9-20.994 1，11.300 6-39.440 9，3.684 2-11.291 4，174.857 8-511.611 8，0-285.127 3，0-48.858 6 mg/g， respectively. The contents of α-pinene，β-pinene，myrcene and γ-terpinene determined by QAMS were 3.296 8-20.994 0，11.300 3- 39.439 7，3.684 1-11.291 1，0-285.126 6 mg/g，respectively. Relative content errors of 4 components as α-pinene determined by 2 methods were all less than 1％ . CONCLUSIONS ： The Δ 基金项目：四川省科技厅应用基础研究项目（No.2021YJ0114）； established GC-QAMS method is simple ，rapid，accurate and 泸州市重点科技项目 [No.2011-S-31（3/3）]；合江县人民政府—西南医科大学战略合作项目（No.2018-HJXNYD-2） repeatable，and can be used for quantitative analysis and ＊硕士研究生。研究方向：中药制备工艺及质量评价。电话： quality control of volatile oil from C. medica . 0830-3162291。E-mail：493359958@qq.com
期刊：	2021年第32卷第16期
作者：	罗忻昳，李培，何兵，张春，张丹，田吉
AUTHORS：	LUO Xinyi，LI Pei，HE Bing，ZHANG Chun，ZHANG Dan，TIAN Ji
关键字：	佛手挥发油；气相色谱法；一测多评法；含量测定
KEYWORDS：	Volatile oil from Citrus medica ；GC；QAMS；
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