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目的 :建立顶空毛细管气相色谱法,测定异丙托溴铵中甲醇、丙酮、异丙醇、二氯甲烷、乙酸乙酯、三氯甲烷、甲苯等7种有机溶剂残留量。方法 :色谱柱:DM-624(聚乙二醇PEG-20M)毛细管柱(30.0m×0.53mm,3.00μm);载气:氮气,流速为2.0mL·min-1;柱温:程序升温,初始温度为40℃,保持5min,然后以6℃·min-1升温到150℃,再以50℃·min-1升温到230℃,保持3min;检测器:氢火焰离子化检测器,温度为250℃;进样口温度:240℃;顶空进样量:1.0mL。结果 :甲醇、丙酮、异丙醇、二氯甲烷、乙酸乙酯、三氯甲烷和甲苯分别在15.02~900.92mg·L-1(r=0.9999)、21.03~1262.00mg·L-1(r=0.9999)、21.30~1278.16mg·L-1(r=0.9999)、7.80~468.25mg·L-1(r=0.9998)、22.22~1332.97mg·L-1(r=0.9999)、0.31~18.79mg·L-1(r=0.9992)和3.48~209.02mg·L-1(r=0.9998)范围内线性关系良好,平均回收率分别为98.1%(RSD=0.19%)、100.1%(RSD=1.08%)、101.4%(RSD=1.03%)、98.1%(RSD=0.40%)、98.1%(RSD=1.55%)、98.9%(RSD=3.08%)和101.8%(RSD=2.12%)。结论 :该方法简便、灵敏、重复性好,结果准确,适用于异丙托溴铵中残留有机溶剂的检测。
OBJECTIVE: To establish a headspace capillary gas chromatographic method for the determination of the residues of seven kinds of organic solvents such as methanol, acetone, isopropanol, dichloromethane, ethyl acetate, chloroform and toluene in ipratropium bromide. Methods: The column was DM-624 (PEG-20M) capillary column (30.0m × 0.53mm, 3.00μm). The carrier gas was nitrogen and the flow rate was 2.0mL · min-1. The initial temperature was 40 ℃, kept for 5min, then heated to 150 ℃ at 6 ℃ · min-1, and then heated to 230 ℃ at 50 ℃ · min-1 for 3min; detector: hydrogen flame ionization detector, temperature 250 ° C; inlet temperature: 240 ° C; headspace sample volume: 1.0 mL. The results showed that methanol, acetone, isopropanol, methylene chloride, ethyl acetate, chloroform and toluene were in the range of 15.02-900.92 mg · L -1 (r = 0.9999) and 21.03-1262.00 mg · L -1 (r = 0.9999), 21.30-1278.16 mg · L -1 (r = 0.9999), 7.80-468.25 mg · L -1 (r = 0.9998), 22.22-1332.97 mg · L -1 (r = 0.9999) The linearity was good in the range of L-1 (r = 0.9992) and 3.48-290.02 mg · L-1 (r = 0.9998) with an average recovery of 98.1% (RSD = 0.19%) and 100.1% (RSD = 1.08% , 101.4% (RSD = 1.03%), 98.1% (RSD = 0.40%), 98.1% (RSD = 1.55%), 98.9% (RSD = 3.08%) and 101.8% (RSD = 2.12%). Conclusion: The method is simple, sensitive, reproducible and accurate. It is suitable for the determination of residual organic solvent in ipratropium bromide.