摘要
目的:建立测定半夏止咳糖浆中挥发性成分(-)-薄荷酮和薄荷脑的方法,并对市售65批半夏止咳糖浆中上述两个成分进行含量测定。方法:采用顶空气相色谱法。色谱柱为Agilent HP-FFAP气相色谱柱(30 m×0.25 mm×0.25μm);程序升温:初始温度90℃,保持2 min,以每分钟3℃的速率升温至140℃,保持6 min;再以每分钟30℃的速率升温至200℃。进样口温度:200℃;检测器温度:250℃;载气为氮气;分流比:10∶1;顶空瓶平衡温度:80℃;平衡时间:20 min。结果:(-)-薄荷酮和薄荷脑分别在0.1839~9.1950μg·mL^-1和0.555~22.2μg·mL^-1范围内线性关系良好;精密度、稳定性、重复性试验的RSD均小于2.5%;加样回收率分别为96.13%(RSD=1.44%,n=6)和98.26%(RSD=2.44%,n=6)。结论:抽样结果表明65批次半夏止咳糖浆中两个成分的含量某些厂家的差异较大。有必要更新该制剂的质量标准,增加气相含量测定项目,加强对其质量控制。建立的质量标准简便可行,可用于半夏止咳糖浆的质量控制。
Objective:To establish a method for determination of(-)-menthone and menthol in Banxiazhike syrup,and the contents of(-)-menthone and menthol in 65 batches of Banxiazhike syrup were determined.Methods:HS-GC was adopted.The test was performed in Agilent HP-FFAP gas phase column(30 m×0.25 mm×0.25 mm)under the programmed temperature condition.The programmed temperature procedure was as:keeping initial 90℃for 2minutes;increasing to 140℃at 3℃/min and maintaining 140℃for 6 minutes;then increasing to 200℃at 30℃/min.The injection temperature was 200℃and detector temperature was 250℃.The carrier gas was nitrogen and the split ratio was 10∶1.The headspace vial balance temperature was 80℃and the balance time was 20 minutes.Results:The linear ranges of(-)-menthone and menthol fell into 0.1839-9.1950μg·mL^-1 and 0.555-22.2μg·mL^-1 respectively,and the average recoveries were 96.13%with RSD as 1.44%(n=6)and 98.26%with RSD as 2.44%(n=6)respectively.All the RSDs of precision,repeatability and stability were less than 2.5%.Conclusion:The test results of 65 batches of Banxia Zhike Syrup showed that there were big differences on contents of(-)-menthone and menthol.It is necessary to improve the specification of Banxia Zhike Syrup and to add the gas phase determination.The quality control of Baixia Zhike Syrup should be strengthened.The established specification is feasible and can be used for quality control of Baixia Zhike Syrup.
作者
牛辰瑾
周军
NIU Chenjin;ZHOU Jun(Tianjin Institute for Drug Control,Tianjin 300070,China)
出处
《中国药品标准》
CAS
2020年第3期274-280,共7页
Drug Standards of China
