文章建立了顶空-气相色谱法测定药用复合硬片中氯乙烯和偏二氯乙烯单体残留量的方法。采用HP-INNOWAX毛细管柱（60 m×0.32 mm×0.5 μm）分离，氢火焰离子化检测器检测，顶空平衡温度80 ℃，平衡时间30 min，柱温50 ℃，分流比10∶1，进样口温度200 ℃，检测器温度为220 ℃。结果表明：氯乙烯和偏二氯乙烯在0.05~5.0 μg范围内线性关系良好（r >0.999），平均回收率分别为102.1%、101.3%，相对偏差（RSD）分别为1.7%、1.9%，氯乙烯的检出限为0.020 μg/g，偏氯乙烯的检出限为0.025 μg/g。此方法操作简便、结果准确、灵敏度高，可用于药用复合硬片中氯乙烯和偏二氯乙烯单体残留量的测定。

The article establishes a headspace gas chromatography method for the determination of vinyl chloride and vinylidene chloride monomer residues in medicinal composite sheet. The separation was performed by HP-INNOWAX capillary column (60 m×0.32 mm×0.5 μm), and hydrogen flame ionization detector was used for testing. Headspace equilibrium temperature was 80 ℃, equilibrium time was 30 min. The column temperature was 50 ℃. The split ratio was 10∶1. The inlet temperature was 200 ℃, and the FID detector temperature was 220 ℃. The results showed that the linear relationship between vinyl chloride and vinylidean chloride was good (r >0.999) in the range of 0.05~5.0 μg. The average recoveries were 102.1%, 101.3%, and the relative standard deviations (RSD) were 1.7% and 1.9%, respectively. The detection limit of vinyl chloride was 0.020 μg/g, and the detection limit of vinylidene chloride was 0.025 μg/g. This method is characterized by its simplicity in operation, accuracy of results, and high sensitivity, and is applicable for the determination of residual vinyl chloride and vinylidene chloride monomer in medicinal composite sheet.