| 引用本文: | 程磊,李玉兰,唐洋明,毕开顺,陈晓辉,王铁杰.GC测定胸腺法新中5种有机溶剂残留量[J].中国现代应用药学,2013,30(6):657-660. |
| CHENG Lei,LI Yulan,TANG Yangming,BI Kaishun,CHEN Xiaohui,WANG Tiejie.Determination of Five Residual Organic Solvents in Thymalfasin by GC[J].Chin J Mod Appl Pharm(中国现代应用药学),2013,30(6):657-660. |
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| 摘要: |
| 目的 建立胸腺法新中5种有机溶剂残留量的气相测定方法。方法 采用气相色谱法，FID检测器，DB-624毛细管色谱柱，以正丁醇为内标进行测定。结果 5种有机溶剂完全分离(R>2.0)，理论板数均>10 000，样品不干扰5种残留溶剂的测定，线性关系良好，甲醇、乙腈、二氯甲烷、吡啶、N,N-二甲基甲酰胺(DMF)的线性范围分别为30~480 μg·mL-1(r=0.999 8)，4.1~65.6 μg·mL-1(r=0.999 9)，6.0~96 μg·mL-1(r=0.999 2)，2.0~32.0 μg·mL-1(r=0.999 3)，8.8~141 μg·mL-1(r=0.999 9)。5种有机溶剂的平均回收率(n=9)依次为99.6%，100.8%，99.8%，100.8%，99.0%。结论 该方法简单、灵敏、准确、耐用性好，适用于胸腺法新中5种有机溶剂残留量的测定。 |
| 关键词: 胸腺法新 有机溶剂残留量 内标法 气相色谱法 |
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| Determination of Five Residual Organic Solvents in Thymalfasin by GC |
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CHENG Lei1, LI Yulan2, TANG Yangming3, BI Kaishun1, CHEN Xiaohui1, WANG Tiejie2
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1.School of Pharmacy, Shenyang Pharmaceutical University, Shenyang 110016, China;2.Shenzhen Institute for Drug Control, Shenzhen 518057, China;3.Shenzhen Hybio Pharmaceutical Corporation, Shenzhen 518057, China
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| Abstract: |
| OBJECTIVE To develop a GC method for the determination of five residual organic solvents in thymalfasin. METHODS The five residual organic solvents were determined by GC with FID detector, on DB-624 capillary GC column, with n-butyl alcohol as internal standard. RESULTS The five residual organic solvents were completely separated (R>2.0), and theoretical plate numbers were all above 10 000. Thymalfasin sample had no interference with the detection of the five residual organic solvents. The method had a good linearity and the liner range of methanol, acetonitrile, dichloromethane, pyridine and DMF were 30-480 μg·mL-1(r=0.999 8), 4.1-65.6 μg·mL-1(r=0.999 9), 6.0-96 μg·mL-1(r=0.999 2), 2.0-32.0 μg·mL-1(r=0.999 3), 8.8-141 μg·mL-1(r=0.999 9), respectively. The recoveries (n=9) of above five organic solvents were 99.6%, 100.8%, 99.8%, 100.8%, 99.0%, respectively. CONCLUSION The method is simple, sensitive, and accurate with good durability. It can be used for the determination of the five residual organic solvents in thymalfasin. |
| Key words: thymalfasin residual organic solvent internal standard method GC |
