GC测定甲苯咪唑中的残留溶剂

Determination of Residual Organic Solvents in Mebendazole by GC

关键词:  气相色谱法  顶空  原料药  甲苯咪唑  残留溶剂

Key words:  gas chromatography  head space  active pharmaceutical ingredients  mebendazole  residual solvents

摘要:

目的 采用顶空气相色谱法测定甲苯咪唑原料药中的有机溶剂残留量。方法 以DMF-H₂O（2︰1）溶液为样品溶剂，选用PerkinElmer气相色谱仪，配备顶空进样器和FID检测器，Agilent DB-624毛细管柱为分析柱，外标法测定。结果 甲醇、乙醇、异丙醇、三氯甲烷和甲苯分别在18.7~224，46.9~562，46.9~562，1.50~17.9，2.81~33.8 μg·mL^-1内线性关系良好（r>0.999）；各组分检出限分别为0.19，0.10，0.11，0.18，0.08 μg·mL^-1；各组分回收率为90.0%~110.0%。结论 该方法准确、灵敏、可靠，可用于甲苯咪唑有机残留溶剂的测定。

Abstract:

OBJECTIVE To establish a headspace gas chromatography method for determination of residual solvents in mebendazole active pharmaceutical ingredients. METHODS The samples were dissolved in DMF-H₂O(2︰1). PerkinElmer gas chromatography with headspace sampling and FID detector was selected. Agilent DB-624 capillary column was used as analytical column. External standard method was used to determine the content. RESULTS A good linear correlation of methanol, alcohol, isopropanol, trichloromethane and toluenethe were shown at the range of 18.7-224, 46.9-562, 46.9-562, 1.50-17.9, 2.81-33.8 μg·mL^-1(r>0.999), respectively. Detection limit of each components were 0.19, 0.10, 0.11, 0.18, 0.08 μg·mL^-1. Recovery range were 90.0%-110.0%. CONCLUSION With good accuracy, sensitivity and reliability, the method can be used for the determination of the residual organic solvents in mebendazole.