提出了气相色谱-质谱法测定感冒颗粒中山梨酸、脱氢乙酸、苯甲酸、对羟基苯甲酸甲酯、对羟基苯甲酸乙酯、对羟基苯甲酸丙酯、对羟基苯甲酸丁酯等7种防腐剂含量的方法。样品经盐酸(1+1)溶液酸化后用乙醚提取,所得提取液用DB-FFAP色谱柱分离,在选择离子监测模式下测定,以正十一烯酸为内标物。7种防腐剂的峰面积与质量浓度在1.0~40.0 mg·L-1范围内呈线性关系,检出限(3S/N)在0.03~0.30 mg·kg-1之间。在5.0,20.0 mg·L-1两个浓度水平进行加标回收试验,7种防腐剂的回收率在82.5%~88.5%之间,相对标准偏差(n=5)在0.80%~6.7%之间。

A method of GC-MS for the determination of seven preservatives, i.e. sorbic acid , benzoic acid , dehydroacetic acid , methyl paraben , ethyl paraben , propyl paraben and butyl paraben in granulated drugs for common cold was proposed. The drug sample was acidified with HCl (1+1) solution and extracted with ethyl ether. The extracts were separated on DB-FFAP column, and determined under selected ion monitoring mode in MS. n-Undecylenic acid was used as internal standard. Linear relationships between values of peak area and mass concentration of the 7 preservatives were kept in the same range of 1.0-40.0 mg·L-1, with detection limits (3S/N) in the range of 0.03-0.30 mg·kg-1. Tests for recovery were made at the concentration levels of 5.0 and 20.0 mg·L-1 of the mixed standards, values of recovery found were in the range of 82.5%-88.5% with RSD′s (n=5) in the range of 0.80%-6.7%.