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0.5μL,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、0.0342-0.2396 mg/mL(r均大于0.999);检测限分别为4.82、7.89、4.01、4.54、5.53、2.47μg/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(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0.9978、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、0-48.8586 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3.2968-20.9940、11.3003-39.4397、3.6841-11.2911、0-285.1266 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。
OBJECTIVE:To establish a method for simultaneous determination ofα-pinene,β-pinene,myrcene,limonene,γ-terpinene andα-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 0.5μL with split ratio of 35∶1.Using limonene as internal reference,relative correction factors ofα-pinene,β-pinene,myrcene andγ-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 ofα-pinene,β-pinene,myrcene,limonene,γ-terpinene andα-terpineol were 0.0305-0.2138,0.0666-0.4660,0.0218-0.1523,0.7652-5.3564,0.3873-2.7108,0.0342-0.2396 mg/mL(all r>0.999).The limits of detection were 4.82,7.89,4.01,4.54,5.53,2.47μg/mL,and the limits of quantification were 15.34,25.91,13.69,15.70,18.68,8.36μg/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 ofα-pinene,β-pinene,myrcene andγ-terpinene were 0.9978,1.5307,0.9524 and 1.0255(all RSD<1%).The contents ofα-pinene,β-pinene,myrcene,limonene,γ-terpinene andα-terpineol by ISM were 3.2969-20.9941,11.3006-39.4409,3.6842-11.2914,174.8578-511.6118,0-285.1273,0-48.8586 mg/g,respectively.The contents ofα-pinene,β-pinene,myrcene andγ-terpinene determined by QAMS were 3.2968-20.9940,11.3003-39.4397,3.6841-11.2911,0-285.1266 mg/g,respectively.Relative content errors of 4 components asα-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.
作者
罗忻昳
李培
何兵
张春
张丹
田吉
LUO Xinyi;LI Pei;HE Bing;ZHANG Chun;ZHANG Dan;TIAN Ji(School of Pharmacy,Southwest Medical University,Sichuan Luzhou 646000,China)
出处
《中国药房》
CAS
北大核心
2021年第16期1995-2001,共7页
China Pharmacy
基金
四川省科技厅应用基础研究项目(No.2021YJ0114)
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)。
