论文部分内容阅读
目的建立了顶空气相色谱法测定非索非那定中甲醇、甲苯、正己烷、四氢呋喃、二氯甲烷、乙酸乙酯、二硫化碳、乙醚和乙醇9种有机溶剂的残留量。方法采用HP-FFAP毛细管柱(50m×0.32mm×0.52μm),FID检测器,外标法进行定量。进样口180℃,检测器250℃,柱温45℃保持9min,以10℃/min程序升温至100℃,保持2min,分流比10:1。载气氮气流速:10ml/min;空气350ml/min;柱头压:氢气45ml/min。顶空瓶区域温度:90℃;样品进样阀:100℃,传输管温度:100℃;样品瓶加热平衡时间:10min;进样量:100μl。对分离条件、顶空平衡温度、平衡时间对残留有机溶剂测定的影响进行了研究。结果甲醇、甲苯、正己烷、四氢呋喃、二氯甲烷、乙酸乙酯、二硫化碳、乙醚和乙醇的线性范围分别为1.58～31.60μg(r=0.9997)、1.73～34.60μg(r=0.9993)、6.65～13.30μg(r=0.9964)、1.32～26.40μg(r=0.9998)、2.52～50.40μg(r=0.9971)、2.52～50.40μg(r=0.9986)、2.66～53.20μg(r=0.9961)、1.80～36.00μg(r=0.9974)、1.58～31.60μg(r=0.9984),各组分回收率均在95%～105%内,最低检测限分别为0.79、0.87、0.66、0.89、1.33、0.90、0.72、1.26和0.79μg。结论该方法操作快速、灵敏、准确。
OBJECTIVE To establish a headspace gas chromatographic method for the determination of the residues of nine organic solvents such as methanol, toluene, n-hexane, tetrahydrofuran, methylene chloride, ethyl acetate, carbon disulfide, diethyl ether and ethanol in fexofenadine. Methods HP-FFAP capillary column (50m × 0.32mm × 0.52μm), FID detector and external standard method were used for quantification. Inlet 180 ℃, detector 250 ℃, column temperature 45 ℃ for 9min, with 10 ℃ / min temperature programmed to 100 ℃, hold 2min, split ratio 10: 1. Carrier gas nitrogen flow rate: 10 ml / min; Air 350 ml / min; Head pressure: Hydrogen 45 ml / min. Headspace bottle area temperature: 90 ° C; Sample injection valve: 100 ° C, Transfer tube temperature: 100 ° C; Vial heating equilibration time: 10 min; Injection volume: 100 μl. The effects of separation conditions, headspace equilibrium temperature and equilibrium time on the determination of residual organic solvents were studied. Results The linear ranges of methanol, toluene, n-hexane, tetrahydrofuran, dichloromethane, ethyl acetate, carbon disulfide, ether and ethanol were 1.58-31.60μg (r = 0.9997), 1.73-34.60μg (r = 0.9993) (R = 0.9986), 2.66 ~ 53.20μg (r = 0.9961), 1.32 ~ 26.40μg (r = 0.9998), 2.52 ~ 50.40μg 36.00μg (r = 0.9974), 1.58 ~ 31.60μg (r = 0.9984). The recoveries of all the components were in the range of 95% -105% with the detection limits of 0.79,0.87,0.66,0.89,1.33,0.90,0.72 , 1.26 and 0.79 μg. Conclusion The method is fast, sensitive and accurate.