| 引用本文: | 唐立超,黄剑英,胡猛慎,段营辉,郑淑凤,李玲玲.GC测定甲苯咪唑中的残留溶剂[J].中国现代应用药学,2018,35(7):995-997. |
| TANG Lichao,HUANG Jianying,HU Mengshen,DUAN Yinghui,ZHENG Shufeng,LI Lingling.Determination of Residual Organic Solvents in Mebendazole by GC[J].Chin J Mod Appl Pharm(中国现代应用药学),2018,35(7):995-997. |
|
| 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。 |
| 关键词: 气相色谱法 顶空 原料药 甲苯咪唑 残留溶剂 |
| DOI：10.13748/j.cnki.issn1007-7693.2018.07.010 |
| 分类号:R917 |
| 基金项目: |
|
| Determination of Residual Organic Solvents in Mebendazole by GC |
|
TANG Lichao, HUANG Jianying, HU Mengshen, DUAN Yinghui, ZHENG Shufeng, LI Lingling
|
|
Xiamen Institution for Food and Drug Quality Control, Xiamen 361012, China
|
| 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. |
| Key words: gas chromatography head space active pharmaceutical ingredients mebendazole residual solvents |
