YJLS原料药中5种有机溶剂残留量顶空气相色谱检测方法的研究  

Determination and Verification of Five Residual Organic Solvents in Raw Materials by Headspace Gas Chromatography

作　　者：王莉莉 贾成华 马挺 WANG Li-li;JIA Cheng-hua;MA Ting(Inspectionand Testing Officeof Mentougou Bureauof Market Supervisionand Administration,Beijing102300,China;Beijing Quality Supervision Office,Centerfor Quality Supervision of EnergyforJoint Logistic Support Force,Beijing100010,China;The 19th Rest Homefor Retired Military Officers,Beijing Garrison Command,Beijing 100143,China)

机构地区：[1]北京市门头沟区市场监督管理检验检测所,北京102300 [2]联勤保障部队军需能源质量监督总站北京质量监督站,北京100010 [3]北京卫戍区第十九离职干部休养所,北京100143

出　　处：《解放军药学学报》2023年第4期321-324,共4页Pharmaceutical Journal of Chinese People's Liberation Army

摘　　要：目的应用顶空气相色谱法建立5种有机溶剂(四氢呋喃、正庚烷、乙腈、异丙醇和甲苯)残留量检测方法,并测定原料药YJLS中5种有机溶剂的含量。方法HS-GC色谱柱(Agilent HP-INNOWAX聚乙二醇为填料的气相色谱柱);柱温采用程序升温;检测器为氢火焰离子化检测器,载气为高纯氮气,优化设置顶空进样量、顶空平衡温度和顶空平衡时间等条件。对原料药YJLS合成工艺中用到的四氢呋喃、正庚烷、乙腈、异丙醇和甲苯等5种有机溶剂,建立气相色谱条件进行残留检测方法,并对该方法进行验证。结果5种有机溶剂在建立的色谱条件下均能完全分离,浓度分别在0.637~57.280、0.649~394.960、0.612~35.200、0.617~400.400、0.683~75.360μg·ml^(-1)范围内具有良好的线性;相关系数分别为0.9999、0.9986、0.9999、0.9999、0.9999;各溶剂回收率范围为80.0%~120.0%,回收率的RSD≤10.0%;精密度的相对标准偏差均小于10%,精密度和准确度结果良好。结论本法可以准确检测YJLS原料药中的四氢呋喃、正庚烷、乙腈、异丙醇和甲苯的残留量。Objective To establish a method for detecting the five types of residual organic solvents and determine their contents in the raw material YJLS.Methods Headspace gas chromatography was performed on an Agilent HP-INNOWAX(polyethyleneglycol as the stationary phase)capillary column using temperature programming.The FID detector was used and the carrier gas was nitrogen.Conditions such as the headspace injection volume,headspace equilibrium temperature and headspace equilibrium time were optimized.Headspace gas chromatography was used to detect the residual solvents of tetrahydrofuran,nheptane,acetonitrile,isopropyl alcohol and toluene used in the synthesis of the raw material YJLS before the method was verified.Results The five types of residual organic solvents were separated completely.The results showed that there was a very good linearity in the range of 0.6368-57.2800μg·ml^(-1) for tetrahydrofuran(r=0.9999),0.649-394.960μg·ml^(-1) for n-heptane(r=0.9986),0.612-35.200μg·ml^(-1) for acetonitrile(r=0.9999),0.617-400.400μg·ml^(-1) for isopropyl alcohol(r=0.9999)and 0.683-75.360μg·ml^(-1) for toluene(r=0.9999).The recoveries ranged from 80.0%to 120.0%,while all the RSDs were below 10%.This method could ensure good precision and accuracy.Conclusion This method can accurately detect the residual solvents of tetrahydrofuran,n-heptane,acetonitrile,isopropyl alcohol and toluene in YJLS.

关 键 词：原料药 有机溶剂残留量 顶空气相色谱 方法学验证 

分 类 号：R927[医药卫生—药学]