气相色谱-质谱法测定葛根和丹参提取回收乙醇中5种挥发性杂质含量  

Content Determination of Five Kinds of Volatile Impurities in Recycled Ethanol After Extracling Pueraria Lobata and Salvia Miltiorrhiza by Gas Chromatography-Mass Spectrometry

作　　者：辜俊鑫 史谢飞[2] 李斌[2] 张学霞 GU Junxin;SHI Xiefei;LI Bin;ZHANG Xuexia(Beijing Tongrentang Technologies Chengdu Co.,Ltd.,Chengdu,Sichuan,China 610100;National Institute of Measurement and Testing Technology,Chengdu,Sichuan,China 610021)

机构地区：[1]北京同仁堂科技发展成都有限公司,四川成都610100 [2]中国测试技术研究院,四川成都610021

出　　处：《中国药业》2021年第17期73-76,共4页China Pharmaceuticals

摘　　要：目的建立测定葛根、丹参提取回收乙醇中甲醇、苯、乙醛、乙缩醛、4-甲基-2-戊醇5种挥发性杂质含量的气相色谱-质谱法。方法色谱柱为Agilent DB-624 UI柱(60 m×250μm,1.4μm),载气为氦气(纯度≥99.999%),流速为1.0 m L/min,分流比为10∶1,进样口温度为230℃,检测器为质谱仪,离子化能量为70 e V,溶剂延迟为4.4 min,柱温为程序升温(40℃保持10 min,以5℃/min的速率升至120℃,再以40℃/min的速率升至220℃并保持3 min),扫描方式为离子监测。结果甲醇、苯、乙醛、乙缩醛、4-甲基-2-戊醇5种挥发性杂质均在各自质量浓度范围内与定量离子峰面积线性关系良好(r≥0.9990,n=7);检测限介于0.02~3.00 mg/L,定量限介于0.05~12.00 mg/L;精密度、稳定性、重复性试验结果的RSD均小于6%(n=6);平均加样回收率介于89.56%~95.20%,RSD介于0.76%~5.08%(n=6)。结论该方法结果准确,精密度较高,重复性好,可用于葛根和丹参提取回收乙醇中挥发性杂质的含量测定。回收乙醇应规定使用周期或循环使用次数,以确保药品质量。Objective To establish a gas chromatography-mass spectrometry(GC-MS)method for the determination of five kinds of volatile impurities of methanol,benzene,acetaldehyde,acetal and 4-methyl-2-pentanol in recycled ethanol after extracting Pueraria lobata and Salvia miltiorrhiza.Methods The chromatographic column was Agilent DB-624 UI column(60 m×250μm,1.4μm),the carrier gas was helium(purity≥99.999%),the flow rate was 1.0 m L/min,the split ratio was 10∶1,the inlet temperature was 230℃,the detector was mass spectrometer,the ionization energy was 70 eV,the time of solvent delay was 4.4 min,and the column temperature was programmed,which was maintained at 40℃for 10 min,heated to 120℃at the rate of 5℃/min,then heated to 220℃at the rate of 40℃/min,and then maintained for 3 min.The scanning method was ion monitoring.Results The five kinds of volatile impurities of methanol,benzene,acetaldehyde,acetal and 4-methyl-2-pentanol had a good linear relationship with the quantitative ion peak area within their respective mass concentration range(r≥0.9990,n=7).The limit of detection(LOD)was in the range of0.02-3.00 mg/L and the limit of quantitation(LOQ)was in the range of 0.05-12.00 mg/L.The RSDs of precision,stability and repeatability tests were less than 6%(n=6).The average recoveries of five kinds of volatile impurities were in the range of 89.56%-95.20%with RSDs of 0.76%-5.08%(n=6).Conclusion The method has high accuracy,precision and good repeatability,which can be used for the content determination of volatile impurities in recycled ethanol after extracting Pueraria lobata and Salvia miltiorrhiza.The use cycle or recycling times of recycled ethanol should be specified to ensure the quality of drugs.

关 键 词：回收乙醇 挥发性杂质 气相色谱-质谱法 甲醇 苯 乙醛 乙缩醛 4-甲基-2-戊醇 含量测定 

分 类 号：R932[医药卫生—生药学] R284.1[医药卫生—药学]