毛细管色谱法测定替莫唑胺酯中的有机溶剂残留量

目的建立毛细管气相色谱法测定替莫唑胺酯中的有机溶剂残留量。方法采用INNOWax毛细管气相色谱柱、FID检测器,以乙腈为内标进行测定。结果正己醇、丙酮、乙酸乙酯、异丙醇、正己烷、吡啶的线性范围分别为25～400μg.L-1(r=0.999 6)、25～400μg.L-1(r=0.999 9)、25～400μg.L-1(r=0.999 9)、25～400μg.L-1(r=0.999 7)、1.45～23.2μg.L-1(r=0.999 8)和1～16μg.L-1(r=0.999 3);正己醇、丙酮、乙酸乙酯、异丙醇、正己烷、吡啶的平均回收率分别为99.7%、100.3%、100.2%、100.4%、99.9%和100.3%;RSD分别为1.11%、1.43%、1.47%、1.37%、1.59%和1.47%(n=9)。结论该方法简单、灵敏、准确、重现性好,适用于替莫唑胺酯中的有机溶剂残留量的测定。

Determination of residual organic solvents in temozolomide hexyl ester by capillary gas chromatography

Objective To develop a gas chromatography method for the determination of residual organic solvents in temozolomide hexyl ester. Methods The samples were injected into INNOWax capillary column and analyzed with FID detector using acetonitrile as the internal standard. Results The linear ranges of hexanol, acetone, ethyl acetate, isopropanol, hexane, pyridine were 25-400 μg·L ^-1 ( r = 0.999 6), 25-400 μg·L ^{- 1} (r = 0.999 9), 25-400 μg·L ^{- 1} ( r = 0.999 9), 25-400 μg·L ^-1 ( r = 0.999 7), 1.45-23.2 μg·L ^{- 1} (r = 0.999 8, 1-16 μg·L ^{- 1} ( r = 0.999 3), respectively. The recoveries were 99.7%, 100.3 %, 100.2 %, 100.4%, 99.9 %, 100.3 %; RSD were 1.11 %, 1.43 %, 1.47 % , 1.37 %, 1.59 %, 1.47 % ( n =9), respectively. Conclusions The method is simple, accurate and sensitive with good reproducibility. It can be used for the determination of the residual organic solvents in temozolomide hexyl ester.