摘要
采用顶空气相色谱法,色谱柱为DB-FFAP毛细管柱,顶空平衡温度为85℃,平衡时间为40min,通过程序升温测定了替考拉宁纯化中10种大孔树脂残留溶剂。结果表明,在0.06～1.20μg·mL-1范围内,正己烷、氯苯和二乙烯苯的峰面积与浓度线性关系良好(R分别为0.997 6、0.996 8、0.996 8),平均回收率分别为101.25%、100.84%、101.03%;在0.12～2.40μg·mL-1范围内,丙烯酸乙酯、甲基丙烯酸甲酯、甲苯、二甲苯和苯乙烯线性关系良好(R分别为0.999 9、0.996 2、0.996 8、0.996 9、0.996 8),平均回收率分别为101.38%、101.20%、100.93%、100.87%、100.76%;在0.012～0.240μg·mL-1范围内,苯和1,2-二氯乙烷线性关系良好(R分别为0.996 6、0.996 2),平均回收率分别为101.29%、102.16%。该方法操作简单、准确度高、重复性好,可用于替考拉宁树脂残留物的质量控制。
We determined ten residual solvents of macroporous adsorbent resin in the purification of Teicoplanin by headspace gas chromatography under the conditions as follows:using DB FFAP capillary column,at the headspace equilibrium temperature of 85℃,for the headspace equilibrium time of 40 min,and using temperature programming.The results show that the calibration curves of hexyl hydride,chlorobenzene,and diethylene benzene show good linear relationship within the range of 0.06^-1.20μg·mL^-1(R=0.997 6,0.996 8,0.996 8),and the average recoveries are 101.25%,100.84%,and 101.03%,respectively.Moreover,the calibration curves of ethyl acrylate,methacrylate,methylbenzene,xylene,and styrene show good linear relationship within the range of 0.12-2.40μg·mL^-1(R=0.999 9,0.996 2,0.996 8,0.996 9,0.996 8),and the average recoveries are 101.38%,101.20%,100.93%,100.87%,and 100.76%,respectively.Furthermore,benzene and 1,2 dichloroethane have good linear relationship within the range of 0.012-0.240μg·mL^-1(R=0.996 6,0.996 2),and the average recoveries are 101.29%and 102.16%,respectively.The method is simple,accurate,and repetitive,which can be used to control the resin residues in Teicoplanin.
作者
邵昉
李丽红
李晓露
任风芝
李宁
张雪霞
耿文飞
SHAO Fang;LI Lihong;LI Xiaolu;REN Fengzhi;LI Ning;ZHANG Xuexia;GENG Wenfei(National Engineering Research Center of Microbial Medicine,Hebei Industry Microbial Metabolic Engineering&Technology Research Center,State Key Laboratory of Antibody Research&Development,Shijiazhuang 050015,China)
出处
《化学与生物工程》
CAS
2019年第1期64-68,共5页
Chemistry & Bioengineering
基金
石家庄市专利实施产业化项目(201803)
关键词
顶空气相色谱法
替考拉宁
大孔吸附树脂
残留溶剂
headspace gas chromatography
Teicoplanin
macroporous adsorbent resin
residual solvent
作者简介
邵昉(1985-),女,河北张家口人,工程师,主要从事药品质量研究,Email:267257334@qq.com;并列第一作者,李丽红(1979-),女,高级工程师,主要从事药品质量研究,Email:llhong21@163.com;通讯作者:张雪霞,正高职高级工程师,Email:zhangxuexia@163.com;通讯作者:耿文飞,正高职高级工程师,Email:wenfeig@163.com
