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目的:完善复方薄荷脑醑质量标准。方法:薄荷脑及苯酚含量测定方法:色谱柱:HP-FFAP(30 m×0.53mm×1.00μm);柱温:初始温度60℃,保持4 min,以2℃/min的速率升温至100℃,再以10℃/min的速率升温至230℃,保持1 min;进样口温度:250℃;检测器温度:250℃;分流比:15∶1。乙醇量测定方法:色谱柱:DB-624(30 m×0.53 mm×3.00μm);柱温:起始温度为40℃,保持2 min,以3℃/min的速率升温至65℃,再以25℃/min的速率升温至200℃,保持10 min;进样口温度200℃;检测器(FID)温度220℃;分流比为1∶1。结果:薄荷脑的线性范围是0.048~0.960 mg/m L,回归方程为Y_1=0.16824X_1-0.01204(r_1=0.9999),平均加样回收率为101.17%(RSD=0.57%);苯酚的线性范围是0.08~1.60 mg/m L,回归方程为Y_2=0.23601X_2+0.01488(r_2=0.9999),平均加样回收率为100.78%(RSD=0.62%);乙醇的线性范围是0.01%~0.25%,回归方程为Y_3=1.0050X_3+0.0732(r_3=1.000),平均加样回收率为101.22%(RSD=0.1%)。结论:该方法简便,结果准确,可用于复方薄荷脑醑中薄荷脑、苯酚及乙醇的含量测定。
Objective: To improve the quality standards of compound menthol. Methods: The content of menthol and phenol was determined by column chromatography with HP-FFAP (30 m × 0.53 mm × 1.00 μm). The column temperature was kept at 60 ℃ for 4 min and the temperature was increased to 100 ℃ at 2 ℃ / min The temperature was raised to 230 ° C at a rate of 10 ° C / min for 1 min. The temperature of the inlet was 250 ° C. The detector temperature was 250 ° C. The split ratio was 15: 1. Method for determining the amount of ethanol: column: DB-624 (30 m × 0.53 mm × 3.00 μm); column temperature: starting temperature of 40 ° C., holding for 2 min, raising temperature to 65 ° C. at a rate of 3 ° C./min The temperature was raised to 200 ° C at a rate of 25 ° C / min for 10 min; the inlet temperature was 200 ° C; the temperature of the detector (FID) was 220 ° C; and the split ratio was 1: 1. Results: The linear range of menthol was 0.048-0.960 mg / m L, the regression equation was Y_1 = 0.16824X_1-0.01204 (r_1 = 0.9999), the average recovery was 101.17% (RSD = 0.57%). The linear range of phenol The average recovery was 100.78% (RSD = 0.62%); the linear range of ethanol was 0.01% -0.25%, and the linear range of ethanol was 0.01% -0.25% The regression equation was Y_3 = 1.0050X_3 + 0.0732 (r_3 = 1.000). The average recovery was 101.22% (RSD = 0.1%). Conclusion: The method is simple and accurate. It can be used for the determination of menthol, phenol and ethanol in compound menthol.