一测多评法同时测定连翘挥发油中4种有效成分的含量

Simultaneous Determination of 4 Kinds of Effective Components in Volatile Oil of Forsythia suspensa by QAMS

目的:建立同时测定连翘挥发油中α-蒎烯、β-蒎烯、柠檬烯和α-松油醇含量的方法。方法:采用气相色谱法进行测定。色谱柱为HP-5毛细管色谱柱,程序升温,进样口温度为230℃,检测器温度为250℃,分流进样(分流比为8∶1),空气流速为300mL/min,氢气流速为30mL/min,尾吹气流速为30mL/min,进样体积为1μL。以柠檬烯为内参物,建立α-蒎烯、β-蒎烯、α-松油醇的相对校正因子,分别采用不同色谱仪和色谱柱以及待测成分色谱峰定位考察相对校正因子及相对保留时间的重现性;以一测多评法计算4种成分的含量,同时将其与外标法测定结果进行比较。结果:α-蒎烯、β-蒎烯、柠檬烯、α-松油醇检测质量浓度的线性范围分别为16.5~990.0、38.1~2287.5、8.2~491.2、2.4~142.5μg/mL(r≥0.9991);精密度、重复性、稳定性试验的RSD均小于3%(n=6);平均回收率为99.7%~105.5%(RSD<4%,n=9)。相对于柠檬烯(1.00),α-蒎烯、β-蒎烯、α-松油醇的相对校正因子平均值分别为0.91、0.86、1.11(n=3);其相对保留时间分别为0.69~0.74、0.81~0.86、1.25~1.35(RSD<3%,n=3);在不同色谱仪或色谱柱条件下其相对校正因子的RSD为0.21%~4.65%(n=6)。采用上述方法测得4种成分的含量与外标法测定结果基本一致(相对误差绝对值均小于7%)。结论:一测多评法可用于连翘挥发油中4种有效成分的同时测定。

OBJECTIVE: To establish a method for simultaneous determination of α-pinene,β-pinene, limonene and α-terpineol in volatile oil of Forsythia suspensa. METHODS:GC method was adopted. The determination was performed on HP-5 capillary column through temperature-programmed route. The inlet temperature was 230 ℃,and detector temperature was 250 ℃;split sampling was applied(split ratio of 8 ∶ 1);the air flow rate was 300 mL/min,the hydrogen flow rate was 30 mL/min, the tail gas flow rate was 30 mL/min,and the injection volume was 1 μL. Using limonene as internal reference,relative correction factors of α-pinene,β-pinene and α-terpineol were established, and the reproducibility of relative correction factors were investigated by using different chromatographs and columns,and chromatographic peak location of components was measured. The contents of above components were calculated with QAMS,and then compared with the results of external standard method. RESULTS:The linear range of α-pinene,β-pinene,limonene and α-terpineol were 16.5-990.0,38.1-2 287.5,8.2-491.2,2.4-142.5 μg/mL,respectively(r≥0.999 1). RSDs of precision,reproducibility and stability tests were all lower than 3%(n=6). Average recoveries were 99.7%-105.5%(RSD<4%,n=9). Compared with limonene(1.00),the average relative correction factors of α-pinene,β-pinene and α-terpineol were 0.91,0.86 and 1.11(n=3);relative retention time were 0.69-0.74,0.81-0.86,1.25-1.35 (RSD<3%,n=3). By using different chromatographs and columns,RSDs of relative correction factors were 0.21%-4.65%(n= 6). Compared with external standard method,determination results of above 4 components were consistent(the absolute value of relative error were all less than 7%). CONCLUSIONS:QAMS can be used for simultaneous determination of 4 kinds of effective components in volatile oil from F. suspensa.