摘要
目的 建立毛细管气相色谱法测定褪黑素类似物AGO中乙醇、乙酸乙酯、二氯甲烷、四氢呋喃、甲苯5种有机溶剂的残留量。方法 采用DB-Wax（30 m×0.45 mm, 0.85 μm）毛细管色谱柱；氢火焰离子化检测器（FID）；程序升温：初始温度45 ℃（维持9 min），以30 ℃·min-1速率升温至200 ℃（维持9 min）；载气为氮气，柱流速为3.5 mL·min^-1；进样口温度：200 ℃；检测器温度：250 ℃；分流直接进样，二甲基亚砜为溶剂，乙腈为内标物，内标法测定残留溶剂的含量。结果 各组分分离完全，在所考察的浓度范围内线性关系良好，其中乙醇、乙酸乙酯、二氯甲烷、四氢呋喃、甲苯的线性范围分别为107.44~1 074.4 μg·mL-1（r=0.999 9），108.24~1 082.4 μg·mL-1（r=0.999 7），18.550~185.50 μg·mL-1（r=0.999 8），14.208~142.08 μg·mL-1（r=0.999 4），19.074~190.74 μg·mL-1（r=0.999 9），平均回收率为98%~102%。结论 该方法操作简单，精密度好，准确可靠，可用于该药物有机溶剂残留量的测定。
OBJECTIVE To establish a capillary GC method for the determination of residual organic solvents including ethanol, ethyl acetate, methylene chloride, tetrahydrofuran and toluene in melatonin analogue. METHODS The residual organic solvents were separated on DB-Wax capillary column（30 m×0.45 mm, 0.85 μm）. FID was used as detector with a temperature of 250 ℃, and the inlet temperature was 200 ℃. The carrier gas was nitrogen, and the flow rate was 3.5 mL·min-1. The programmed column temperature was set as follows： maintained at 45 ℃ for 9 min and raised to 200 ℃ at the rate of 30 ℃·min-1 followed by holding for 9 min. The sample dissolved in dimethylsulfoxide and acetonitrile was used as the internal standard. The assay of residual solvents was calculated by internal standard method. RESULTS Five residual organic solvents were completely separated. The linear ranges of ethanol, ethyl acetate, methylene chloride, tetrahydrofuran and toluene were 107.44-1 074.4 μg·mL-1（r=0.999 9）, 108.24-1 082.4 μg·mL-1（r=0.999 7）, 18.550-185.50 μg·mL-1（r=0.999 8）, 14.208-142.08 μg·mL-1（r=0.999 4）, 19.074-190.74 μg·mL-1（r=0.999 9）, the average recovery of the preparation were between 98%-102%. CONCLUSION The method is simple, sensitive, accurate, and can be used for the determination of the residual organic solvents in melatonin analogue.
出处
《中国现代应用药学》
CAS
CSCD
2013年第6期645-648,共4页
Chinese Journal of Modern Applied Pharmacy
基金
国家自然科学基金项目(81072613)
十二五国家科技重大专项"重大新药创制"综合性新药研究开发技术大平台(2012ZX09301003-001-010)
