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目的建立测定LS-177中8种有机溶剂残留量的顶空气相色谱法。方法采用DB-624(30 m×530μm,3μm)毛细管柱,经程序升温,以氮气为载气,检测器为氢火焰离子化检测器,采用顶空进样方式。以二甲基亚砜(dimethyl sulfoxide,DMSO)为溶剂,用标准加入法对LS-177中的8种有机溶剂进行定量。结果乙醇、乙腈、二氯甲烷、异丙醚、乙酸乙酯、吡啶、甲苯和氯苯在考察范围内线性关系良好,r为0.999 1~0.999 7,检测限分别为0.17、0.28、0.41、0.033、0.09、0.78、0.073和0.09 mg·L-1。结论本方法可用于LS-177中的溶剂残留量测定。
OBJECTIVE To establish a headspace gas chromatographic method for the determination of eight organic solvents in LS-177. Methods DB-624 (30 m × 530 μm, 3 μm) capillary column was used. The temperature was programmed and nitrogen gas was used as the carrier gas. The detector was hydrogen flame ionization detector and the headspace sampling method was used. Eight organic solvents in LS-177 were quantified by standard addition method using dimethyl sulfoxide (DMSO) as a solvent. Results The calibration curves of ethanol, acetonitrile, methylene chloride, isopropyl ether, ethyl acetate, pyridine, toluene and chlorobenzene showed good linearity in the range of 0.999 1 ~ 0.999 7 and the limits of detection were 0.17,0.28,0.41,0.033 0.09, 0.78, 0.073 and 0.09 mg · L -1, respectively. Conclusion This method can be used for the determination of solvent residues in LS-177.