顶空气相色谱法测定美洛昔康中的3种残留溶剂

Headspace gas chromatography determination of three residual solvents in Meloxicam

目的:建立顶空气相色谱法测定药物美洛昔康中3种残留溶剂的方法。方法:采用DB-624毛细管色谱柱(30 m×0.32 mm,1.8μm);柱温采取程序升温;进样口温度为230℃;FID检测器,检测器温度为250℃;顶空进样,平衡温度为130℃,平衡时间为30 min;以二甲亚砜为溶剂测定美洛昔康原料药中乙醇、N,N-二甲基甲酰胺、二甲苯的残留量。结果:在本文的色谱条件下,各有机溶剂均能得到有效分离,乙醇、N,N-二甲基甲酰胺、二甲苯浓度分别在250～750μg.mL-1(r=0.9990)、44～132μg.mL-1(r=0.9987)、108.5～325.5μg.mL-1(r=0.9993)范围内线性关系良好;平均回收率(n=9)分别为97.2%、101.0%、97.9%,RSD分别为1.7%、2.4%、3.1%。结论:本方法简便、快速、准确,可有效检测美洛昔康中的残留溶剂。

Objective： To establish a headspace gas chromatography method for determination of three residual sol- vents in meloxicam. Methods： The residual solvents in Meloxicam were separated on DB - 624 columns （ 30 m × 0. 32 mm, 1.8 μm） with an FID detector. The injector temperature and the detector temperature were set at 230 ℃ and 250 ℃, respectively. The containers of headspace injector were in equilibrium for 30 min at 130 ℃. The dime-thylsulfoxide （DMSO） was used as the solvent. Results： The detected solvents were separated completely. Good lin- earity of the three solvents were obtained within the range of 250 -750 μg · mL^-1（ r = 0. 9990） ,44 - 132 μg · mL^ -1 （ r = 0. 9987 ）, 108.5 - 325.5 μg · mL^-1 （ r = 0. 9993 ）, respectively. The average recoveries （ n = 9 ） of etha- nol,N,N-dimethylformamide,xylene were 97.2% ,101.0% ,97.9% and the RSDs were 1.7% ,2. 4% ,3.1% ,re-spectively. Conclusion： The established method is simple, rapid, and accurate, which can be used for the determi-nation of residual solvents in meloxicam.