Determination of dichloromethane and trichloromethane residues in ranitidine hydrochloride by headspace liquid phase microextraction coupled with gas chromatography
顶空液相微萃取-气相色谱法测定盐酸雷尼替丁中二氯甲烷和三氯甲烷的残留量

A method for the determination of residual dichloromethane and trichloromethane in ranitidine hydrochloride by headspace liquid phase microextraction coupled with gas chroma-tography (GC) was developed. A homemade device was used to protect the organic drop. The effects of the nature of extraction solvent, extraction time, extraction temperature and micro-drop volume on the extraction efficiency were investigated separately. The optimal experimen-tal conditions were as follows:2 ΜL of n-tridecane as extraction solvent, 30 min of extraction time, 60 ℃ of extraction temperature. The correlation coefficients of linear calibration curve were 0. 973 3 and 0. 972 4 within the concentration ranges of dichloromethane (1-10 μg/g) and trichloromethane (1-10 μg/g), respectively. The detection limits of dichlormethane and tri-chloromethane were 0. 027 3 μg/g and 0. 041 0 μg/g, respectively, the relative standard devia-tions were lower than 4. 36% and 5. 89%, and the recoveries of the method were 93. 6% - 102% and 98.1% -103%, respectively. The method is simple and reliable.