美洛昔康残留DMF、二甲苯的测定

Determination of DMF and dimethyl benzene residual in meloxicam

目的利用顶空法气相色谱建立了美洛昔康中残留溶剂的测定方法。方法FID检测器,色谱柱(30m×0.53mm,膜厚3.0μm,固定液:6%氰丙基苯基-94%二甲基聚硅氧烷),检测器温度:260℃;载气:N2;载气流速:10ml.min-1。结果及结论相邻溶剂峰的分离度不小于1.5;重复进样各溶剂峰面积的RSD均小于5%。二甲苯的检测限:3ppm,DMF的检测限:19.48ppm。

OBJECTIVE To determine DMF and dimethyl benzene residual in meloxicam by headspace gas chromatograph. METHODS The headspace gas chromatograph was equipped with a flame-ionization detector,column（30m×0. 53mm;film ; 3. 0urn, phase： 6% cyanopropylphenyl-940% dimethylpolysiloxane）. Detector temperature was 260℃, carrier gas was Nz and the flow rate of carrier gas was 10ml · min^-1. RESULTS and CONCLUSION The resolution between the close peak was more than 1.5, the relative standard deviation for standard replicate injections was less than 5%. The detection limit of dimethyl ben- zene was 3ppm,and the detection limit of DMF was 19. 48ppm.