顶空毛细管气相色谱法测定美司钠原料和注射液的残留溶剂
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摘要
目的建立美司钠原料及其注射剂中4种残留溶剂的顶空毛细管气相色谱测定方法。方法使用HP-1毛细管气相色谱柱(30m×0.25mm,0.25μm),采用程序升温。初始温度为40℃,保持5min,再以20℃·min-1升温至150℃;进样口温度为200℃;检测器为FID;检测器温度为250℃。顶空进样,平衡温度为75℃,平衡时间为30min。结果同时测定了美司钠原料和注射液中4种残留有机溶剂,甲醇、乙醇、异丙醇和丙酮分离度均在2.0以上,线性范围分别为6.6～66.0(r1=0.999 4),4.9～49.1(r2=0.999 9),5.8～58.0(r3=0.999 5)和8.0～80.0μg·mL-1(r4=0.999 6),平均加样回收率分别为97.3%,98.2%,99.5%和99.1%,RSD值分别为1.9%,2.1%,1.5%和1.7%。结论该方法灵敏、准确,可用于美司钠原料及其注射液中残留溶剂的检测。
Objective To establish a headspace capillary gas chromatography method for the determination of 4residual solvents in mesna crude material and injection.Methods The determination was performed on an HP-1column(30m×0.25 mm,0.25μm)with the initial temperature at 40℃ maintaining for 5min,and then up to 150℃ with a speed of 20℃·min-1 through temperature-programmed route.The inlet temperature was 200℃and the FID was used as a detector which was set at 250℃.Headspace sampling was used with temperature of equilibrium at 75℃and the equilibrium time 30 min.Results 4kinds of organic solvents in mesna crude material and injection were determined simultaneously.The resolution between methanol,ethanol,isopropanol and acetone were all above 2.0and the calibration curves were all with good linearity in the ranges of 6.6-66.0μg·mL-1for methanol(r1=0.999 4),4.9-49.1μg·mL-1 for ethanol(r2=0.999 9),5.8-58.0μg·mL-1 for isopropanol(r3=0.999 5)and 8.0-80.0μg·mL-1for acetone(r4=0.999 6).The average recoveries were 97.3%,98.2%,99.5%and 99.1% with RSD 1.9%,2.1%,1.5%and 1.7%,respectively.Conclusion The method was proved to be accurate,sensitive,and can be used for the detection of residual solvents in crude material and injection.
Objective To establish a headspace capillary gas chromatography method for the determination of 4residual solvents in mesna crude material and injection.Methods The determination was performed on an HP-1column(30m×0.25 mm,0.25μm)with the initial temperature at 40℃ maintaining for 5min,and then up to 150℃ with a speed of 20℃·min-1 through temperature-programmed route.The inlet temperature was 200℃and the FID was used as a detector which was set at 250℃.Headspace sampling was used with temperature of equilibrium at 75℃and the equilibrium time 30 min.Results 4kinds of organic solvents in mesna crude material and injection were determined simultaneously.The resolution between methanol,ethanol,isopropanol and acetone were all above 2.0and the calibration curves were all with good linearity in the ranges of 6.6-66.0μg·mL-1for methanol(r1=0.999 4),4.9-49.1μg·mL-1 for ethanol(r2=0.999 9),5.8-58.0μg·mL-1 for isopropanol(r3=0.999 5)and 8.0-80.0μg·mL-1for acetone(r4=0.999 6).The average recoveries were 97.3%,98.2%,99.5%and 99.1% with RSD 1.9%,2.1%,1.5%and 1.7%,respectively.Conclusion The method was proved to be accurate,sensitive,and can be used for the detection of residual solvents in crude material and injection.
引文
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[15]杨欣,蒙萌,程怡凡,等.顶空气相色谱法测定紫杉醇原料药中的有机溶剂残留量[J].西北药学杂志,2017,32(6):748-750.
[16]崇小萌,胡昌勤.利用中等极性气相色谱系统分析药物残留溶剂[J].药物分析杂志,2014,34(11):2048-2053.
[17]杨明兢,吴盼盼,段玺玉,等.顶空气相色谱法测定TM-2中溶剂残留量[J].沈阳药科大学学报,2015,32(7):523-526,536.
[2] Dorris K,Fouladi M,Davies S M,et al.Severe allergic reactions to thiol--based cytoprotective agents mesna and amifostine in a child with a supratentorial primitive neuroectodermal tumor[J].J Pediatr Hematol Oncol,2011,33(6):e250-e252.
[3] Cutler M J,Urquhart B L,Velenosi T J,et al.In vitro and in vivo assessment of renal drug transporters in the disposition of mesna and dimesna[J].J Clin Pharmacol,2011,52:530-542.
[4]国家药典委员会.中华人民共和国药典临床用药须知:化学药和生物制品卷:2010年版[S].北京:中国医药科技出版社,2010:1337-1338.
[5] YBH03952007,国家食品药品监督管理局药品标准[S].
[6] WS-024(X-017)-95,国家食品药品监督管理局国家药品标准颁布件[S].
[7] WS-250-(X-018)-95(1)(2),国家食品药品监督管理总局国家药品标准颁布件[S].
[8] YBH01942009,国家食品药品监督管理局标准[S].
[9] YBH24302006,国家食品药品监督管理局标准[S].
[10]JX20100098,国家食品药品监督管理局进口药品注册标准[S].
[11]赵平,欧莉,王建塔.美司钠合成工艺的改进[J].贵阳医学院学报,2006,31(6):589,592.
[12]国家药典委员会.中国药典:2015年版:四部[S].北京:中国医药科技出版社,2015:861.
[13]杨昭毅,刘斌.顶空气相色谱法测定利奥西呱原料药中9种残留溶剂的含量[J].中国测试,2017,43(6):42-45.
[14]艾芸,张凡,张亚峰,等.注射用环磷酰胺中残留溶剂的测定[J].西北药学杂志,2017,32(3):299-304.
[15]杨欣,蒙萌,程怡凡,等.顶空气相色谱法测定紫杉醇原料药中的有机溶剂残留量[J].西北药学杂志,2017,32(6):748-750.
[16]崇小萌,胡昌勤.利用中等极性气相色谱系统分析药物残留溶剂[J].药物分析杂志,2014,34(11):2048-2053.
[17]杨明兢,吴盼盼,段玺玉,等.顶空气相色谱法测定TM-2中溶剂残留量[J].沈阳药科大学学报,2015,32(7):523-526,536.