气相色谱法同时测定扎冲十三药材中6种挥发性成分的含量
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篇名: 气相色谱法同时测定扎冲十三药材中6种挥发性成分的含量
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摘要: 目的:建立同时测定扎冲十三药材中丁香酚、甲基丁香酚、异丁香酚、α-细辛脑、木香烃内酯、肉豆蔻醚等6种挥发性成分含量的方法。方法:采用水蒸气蒸馏法提取挥发油,采用气相色谱法测定挥发油中6种成分含量。色谱柱为ov-1701毛细管,氢火焰离子化检测器,载气为氮气,进样口温度为220 ℃,检测器温度为240 ℃,流速为1.0 mL/min,进样量为1 μL,分流比为10 ∶ 1,程序升温。结果:丁香酚、甲基丁香酚、异丁香酚、α-细辛脑、木香烃内酯、肉豆蔻醚检测质量浓度线性范围分别为2.00~12.00、1.00~6.00、0.60~3.60、0.05~0.30、0.05~0.30、0.60~3.60 mg/mL(r均为0.999 9),检测限分别为0.01、0.01、0.02、0.01、0.01、0.01 mg/mL,定量限分别为0.05、0.03、0.06、0.02、0.02、0.03 mg/mL;精密度、稳定性、重复性试验的RSD均小于3%;平均加样回收率为99.33%~100.04%,RSD为0.02%~0.35%(n=6);耐用性试验的RSD均小于5%。结论:本研究所建方法操作简单、重复性好,可用于扎冲十三药材中6种挥发性成分含量的同时测定。
ABSTRACT: OBJECTIVE: To establish a method for simultaneously determining the contents of 6 volatile components such as eugenol, methyl eugenol, isoeugenol, α-asarone, alkaloid and myristyl ether in Zhachong shisan. METHODS:Volatile oil was extracted by steam distillation and analyzed by gas chromatography. The chromatographic column was ov-1701, with hydrogen flame ionization detector. The carrier gas was nitrogen, the inlet temperature was 220 ℃, the detector temperature was 240 ℃, the flow rate was 1.0 mL/min, the injection volume was 1 μL, the split ratio was 10 ∶ 1, with programmed temperature. RESULTS: The linear ranges of eugenol, methyl eugenol, isoeugenol, α-asarone, costunolide and myristyl were 2.00-12.00, 1.00-6.00, 0.60-3.60, 0.05-0.30, 0.05-0.30, 0.60-3.60 mg/mL(r=0.999 9). The detection limits were 0.01, 0.01, 0.02, 0.01, 0.01, 0.01 mg/mL, respectively; the limits of quantification were 0.05, 0.03, 0.06, 0.02, 0.02, 0.03 mg/mL, respectively. RSDs of precision, stability and reproducible tests were all lower than 3%; average recovery rates were 99.33%-100.04%, RSDs were 0.02%-0.35% (n=6); RSDs of durability test were all lower than 5%. CONCLUSIONS: The established method was simple and reproducible. It can be used for simultaneous determination of the contents of 6 volatile components in Zhachong shisan.
期刊: 2019年第30卷第12期
作者: 杨彩静,曹人郦,赵颖,王小凤,刘勋,顾艳丽
AUTHORS: YANG Caijing,CAO Renli,ZHAO Ying,WANG Xiaofeng,LIU Xun,GU Yanli
关键字: 扎冲十三;气相色谱法;含量测定;挥发性成分
KEYWORDS: Zhachong shisan; Gas chromatography; Content determination; Volatile component
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