摘要
目的建立以气相色谱-质谱法测定复方枇杷止咳颗粒中薄荷脑含量的方法,为提高复方枇杷止咳颗粒的质量控制方法提供依据。方法采用Agilent HP-5MS(30m×0.25mm×0.25μm)毛细管柱,以水杨酸甲酯为内标,进样口温度:200℃,采取程序升温(初始温度60℃,保持1min,以10℃/min速率升温至200℃,保持2min),载气为高纯氦气,流速1m L·min^(-1),进样量1μL,分流比5∶1;质谱条件:EI源,轰击电压70eV;离子源温度230℃;辅助接口温度280℃,采用全扫描模式获得对照品溶液的总离子流色谱图,确定特征离子,再进行选择离子检测(SIM)定量,选择m/z 81为薄荷脑的检测离子,通过内标法进行定量分析。结果薄荷脑在0.05768μg·mL^(-1)~5.768μg·mL^(-1)范围内线性关系良好(r=0.9983);平均回收率为103.2%,RSD=1.5%。结论该方法经过方法学验证,可有效地对复方枇杷止咳颗粒的质量进行控制。
OBJECTIVE To establish a GC-MS method for the determination of the menthol in Fufang Pipa Zhike Granules,and to provide the basis for improving the quality control method for Fufang Pipa Zhike Granules. METHODS GC-MS method was adopted. Chromatographic conditions were as follows： the Agilent HP-5 MS column（ 30 m × 0. 25 mm × 0. 25μm） was adopted at the injector temperature of 200℃,the interna1 standard was methyl salicylate,the programmed temperature method（ 60℃ for 1 min,10℃/min to 200℃ for 2 min） was used. Helium gas was used as the carrier gas at a constant flow rate of 1 mL·min^-1,with an injection volume of 1μL（ split ratio of 5∶1）. Mass spectra were taken at 70 eV; the ion-source temperature was 230℃,the auxiliary interface temperature 280℃. The characteristic ions for target compound were determined by full scan mode and SIM,and m/z 81 was the detection ion of mentho1. The quantitative analysis of mentho1 was analyzed with interna1 standard method via GC-MS. RESULTS The 1 inear range of menthol was 0. 05768μg · mL^-1- 5. 768μg · mL^-1（ r =0. 9983）,the average recovery was 103. 2%,RSD = 1. 5%. CONCLUSION The method was validated,and can be used to control the quality of Fufang Pipa Zhike Granules.
作者
张建伟
屈蓉
ZHANG Jian-wei;QU Rong(Taizhou Medical Hi-tech Zone Public Service Platform Center,Taizhou 225300, china;Taizhou Institute for Food and Drug ControI,Taizhou 225300, china)
出处
《海峡药学》
2018年第6期57-60,共4页
Strait Pharmaceutical Journal
