罗忻昳 李培 何兵 张春 张丹 田吉

中圖分类号 R284.1 文献标志码 A 文章编号 1001-0408（2021）16-1995-07

DOI 10.6039/j.issn.1001-0408.2021.16.13

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Agilent DB-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0.5 mL/min，氮气（尾吹）流速为25 mL/min，氢气流速为30 mL/min，空气流速为400 mL/min，进样口温度为250 ℃，检测器温度为280 ℃，程序升温，进样量为0.5 μL，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0.030 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（r均大于0.999）;检测限分别为4.82、7.89、4.01、4.54、5.53、2.47 ?g/mL，定量限分别为15.34、25.91、13.69、15.70、18.68、8.36 ?g/mL;精密度、重复性、稳定性（24 h）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0.997 8、1.530 7、0.952 4、1.025 5（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3.296 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;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3.296 8～20.994 0、11.300 3～39.439 7、3.684 1～11.291 1、0～285.126 6 mg/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。

关键词 佛手挥发油;气相色谱法;一测多评法;含量测定

Simultaneous Determination of 6 Components in Volatile Oil from Citrus medica by GC-QAMS

LUO Xinyi，LI Pei，HE Bing，ZHANG Chun，ZHANG Dan，TIAN Ji（School of Pharmacy， Southwest Medical University， Sichuan Luzhou 646000， China）

ABSTRACT   OBJECTIVE： To establish a method for simultaneous determination 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 ?g/mL， and the limits of quantification were 15.34， 25.91， 13.69， 15.70， 18.68， 8.36 ?g/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 established GC-QAMS method is simple， rapid， accurate and repeatable， and can be used for quantitative analysis and quality control of volatile oil from C. medica.

KEYWORDS   Volatile oil from Citrus medica; GC; QAMS; Content determination

佛手为芸香科植物佛手Citrus medica L. var. sarcodactylis Swingle 的干燥果实，收载于2020年版《中国药典》（一部），具有疏肝理气、和胃止痛、燥湿化痰之功[1]。佛……