建立了氟尼辛葡甲胺原料药中乙酸乙酯、甲醇、异丙醇、乙醇和乙腈有机溶剂残留量的顶空气相色谱分析方法.以HP-FFAP色谱柱(30m×0.32 mm×1.0μm)为分离柱,火焰离子化检测器检测,外标法定量,并考察了顶空平衡温度、平衡时间等对残留有机溶剂测定的影响.实验结果表明,在顶空平衡温度为90℃、平衡时间为30min条件下获得较好的定量结果.乙酸乙酯、甲醇、异丙醇、乙醇和乙腈的线性范围分别为0.40～7.93 mg/L (r=0.999 8)、7.32～146.48 mg/L (r=0.999 6)、4.53～90.61 mg/L(r=0.999 9)、3.62 ～ 72.32 mg/L(r=0.999 8)和2.31～46.24 mg/L(r=0.999 6)；平均回收率范围为95.96％ ～100.31％,精密度(以相对标准偏差计,n=6)为1.97％～3.28％；检出限分别为0.08、0.9、0.2、0.4和0.3mg/L.利用该方法对实际样品氟尼辛葡甲胺原料药中有机溶剂残留量进行了检测.结果表明,该样品中含有异丙醇和乙醇,其含量分别为177.44μg/g与69.32 μg/g.本方法快速、灵敏、准确,适用于氟尼辛葡甲胺原料药中残留溶剂的检测.
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