砂仁挥发油中7种活性成分的含量测定研究

目的：建立同时测定砂仁挥发油中α-蒎烯、莰烯、月桂烯、柠檬烯、樟脑、龙脑、乙酸龙脑酯7种活性成分含量的GC法，用于中药砂仁的质量控制。方法：采用DB-5色谱柱（30 m×0.320 mm×0.25 μm），柱温为程序升温，FID检测器，进样口温度230 ℃，检测器温度250 ℃。其中樟脑、龙脑、乙酸龙脑酯3种单萜类挥发油采用一测多评法进行测定。以乙酸龙脑酯为内参物，分别计算樟脑和龙脑的相对校正因子（RCF），利用RCF测定樟脑和龙脑的含量，其余4种活性成分采用外标法测定。结果：α-蒎烯、莰烯、月桂烯、柠檬烯、樟脑、龙脑、乙酸龙脑酯的线性范围分别为3.380~169.0 mg·mL^-1（r=0.999 8）、13.90~696.0 mg·mL^-1（r=0.999 9）、4.200~210.0 mg·mL^-1（r=0.999 9）、18.20~908 mg·mL^-1（r=0.999 9）、10.50~525.0 mg·mL^-1（r=0.999 9）、9.58~479.0 mg·mL^-1（r=0.999 8）和32.60~1.630×103 mg·mL^-1（r=0.999 9），方法平均回收率（n=6）分别为101.3%（RSD=1.9%）、101.5%（RSD=2.6%）、101.9%（RSD=1.2%）、101.3%（RSD=2.3%）、101.0%（RSD=1.6%）、101.7%（RSD=1.3%）和99.9%（RSD=2.2%）。各批次中药砂仁中α-蒎烯、莰烯、月桂烯、柠檬烯、樟脑、龙脑和乙酸龙脑酯7种成分的含量范围分别为0.117 0~0.430 5、0.450 4~3.734、0.101 0~1.808、0.319 6~3.687、1.660~10.40、0.290 0~1.640和0.454 7~13.16 mg·g^-1。结论：所建立的分析方法简便、快速，专属性强，增加了能反映砂仁临床疗效的质量控制指标，为现有国家标准的完善提供依据。

Objective: To establish a method for the simultaneous determination of α-pinene,camphene,myrcene,limonene,camphor,borneol,bornyl acetate in volatile oil by GC,so as to provide a reference for the quality control of Amomis Fructus.Methods: A DB-5(30 m×0.320 mm×0.25 μm)column was adopted with nitrogen as carrier gas and FID as detector.The column temperature was controlled by program.The inlets temperature was 230 ℃,and the FID detector temperature was 250 ℃.Bornyl acetate was used as the internal reference to get the relative correction factors(RCF)of borneol and camphor in ratios to the reference.The contents of three components in all batches of Amomis Fructus were calculated and the quantitative results were compared by t-test between QAMS and ES method.The other four componenets were determined by ES.Results: Seven compounds had good linear relationship,precision,stability and repeatability according to the requirements of the methodology determination.The linear range of α-pinene,camphene,myrcene,limonene,camphor,borneol and bornyl acetatec were 3.380-169.0 mg·mL^-1(r=0.999 8),13.90-696.0 mg·mL^-1(r=0.999 9),4.200-210.0 mg·mL^-1(r=0.999 9),18.20-908 mg·mL^-1(r=0.999 9),10.50-525.0 mg·mL^-1(r=0.999 9),9.58-479.0 mg·mL^-1(r=0.999 8)and 32.60-1.630×103 mg·mL^-1(r=0.999 9).The average recoveries were 101.3%(RSD=1.9%),101.5%(RSD=2.6%),101.9%(RSD=1.2%),101.3%(RSD=2.3%),101.0%(RSD=1.6%),101.7%(RSD=1.3%)and 99.9%(RSD=2.2%),respectively.The contents of α-pinene,camphene,myrcene,limonene,camphor,borneol and bornyl acetatec in volatile oil were ranged in 0.117 0-0.430 5,0.450 4-3.734, 0.101 0-1.808,0.319 6-3.687,1.660-10.40,0.290 0-1.640 and 0.454 7-13.16 mg·g^-1,respectively.Conclusion: The established method is simple,convenient and with good specificity,and could be used as a valid analytical method to evaluate the intrinsic quality of Amomi Fructus.