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建立了液体顶空气相色谱法测定盐酸马尼地平中有机溶剂残留量。采用 DB-1大口径毛细管柱,以正丙醇为内标进行定量。甲醇、乙醇、异丙醇、乙醚、正丙醇及三氯甲烷的线性范围分别为1．5～61．6μg·mL~(-1)(r=0．9991), 0．4～62．0μg·mL~(-1)(r=0．9994),1．6～64．4μg·mL~(-1)(r=0．9984),1．1～43．6μg·mL~(-1)(r=0．9997)和1．5～63．2μg·mL~(-1)(r=0．9992)；回收率分别为99．9%,103．8%,101．8%,97．7%和98．3%；最低检测限分别为0．02μg·g~(-1),0．04μg·g~(-1),0．02μg·g~(-1), 0．01μg·g~(-1)和0．2μg·g~(-1)。本方法简单、准确、灵敏度及重现性好。
A liquid headspace gas chromatography was developed for the determination of organic solvent residues in manidipine hydrochloride. DB-1 large-diameter capillary column with n-propanol as internal standard for quantitative. The linear ranges of methanol, ethanol, isopropanol, ether, n-propanol and trichloromethane were 1.5 ~ 61.6μg · mL -1 (r = 0.9991) and 0.4 ~ 62 respectively. (R = 0.9994), 1.6 ~ 64.4μg · mL -1 (r = 0.9984), 1.1 ~ 43.6μg · mL ~ (-1) 1) (r = 0.9997) and 1.5 ~ 63.2μg · mL -1 (r = 0.9992) .The recovery rates were 99.9%, 103.8% and 101.8% , 97.7% and 98.3%, respectively. The minimum detection limits were 0.02μg · g -1, 0.02μg · g -1, 0.02μg · g -1, .01 μg · g -1 and 0.2 μg · g -1. The method is simple, accurate, good sensitivity and reproducibility.