尼美舒利中有机溶剂残留量的测定  

Determination of Residual Solvent in Nimesulide

作　　者：李玮玲[1] 赵雪梅[1] 

机构地区：[1]广州市药品检验所,广东广州510160

出　　处：《药学进展》2007年第10期465-468,共4页Progress in Pharmaceutical Sciences

摘　　要：目的:采用顶空-气相色谱法测定尼美舒利中有机溶剂残留量。方法:采用DB-WAX毛细管柱(0.53mm×30m,1μm),柱温为40℃,保持4分钟,然后以每分钟10℃的速率升至90℃,保持2分钟,再以每分钟30℃的速率升至180℃,保持2分钟。氢火焰离子化检测器(FID)温度为250℃,进样口温度为200℃,顶空温度为80℃,保持时间为30分钟,进样时间为0.2分钟,载气为氮气,进样压力为9.6×104Pa。结果:丙酮在78.605～393.025mg/L,乙醇在78.763～393.815mg/L,吡啶在3.114～15.570mg/L范围内线性关系良好。丙酮、乙醇和吡啶的平均回收率分别为100.4%(RSD=1.19%)、102.3%(RSD=1.07%)和97.6%(RSD=1.68%)。结论:本方法简单、结果准确、灵敏度高,可用于尼美舒利中有机溶剂残留量的测定。Objective： To develop headspace gas chromatography, method for the determination of residue solvent in nimesulide. Methods： In the test DB-WAX capillary column （0.53 mm × 30 m, 1μm ） was used. The column temperature was raised by program, the initial temperature was 40℃, maintained for 4 min, raised to 90℃ with a rate of 10 ℃/min, maintained for 2 min, then raised to 180℃ with a rate of 30℃/ min, and maintained for 2 min. The detector temperature was 250℃, the injector temperature was 200℃, and headspace temperature was 80℃, maintained for 30 min. The time for injection was 0.2 min, and the injector pressure was 9.6 × 104 Pa. Results. The calibration curves for acetone, ethanol and pyridine were linear in the range of 78. 605-393.025μg/mL, 78.763-393.815 μg/mL and 3.114-15.570μg/mL, respectively. The average recovery of acetone, ethanol and pyridine was 100.4 % （RSD = 1.19 % ）, 102.3 % （RSD = 1.07 % ） and 97.6 % （ RSD = 1.68 % ）, respectively. Conclusion： The method is simple, precise, sensitive and rapid. It could be applied to control residue solvent of nimesulide.

关 键 词：顶空-气相色谱法 尼美舒利 残留溶剂 

分 类 号：R927[医药卫生—药学]