目的 建立一种定量检测异丙醇消毒剂含量的气相色谱法。方法 采用DB-1气相色谱柱,尺寸为30 m(长)×0.53 mm(内径)×3.00 µm(膜厚)。色谱条件如下:程序升温;以氮气为载气,恒定流速5 ml/min;进样口温度为200 ℃,检测器温度为275 ℃;分流进样,进样量1 µl。对该法进行专属性、准确性、重复性、耐用性验证。结果 异丙醇气体和正丁醇气体完全分离,分离度为25.4。该法在考察范围内线性良好,决定系数为0.999 977。正丁醇稀释液色谱图中没有干扰峰出现。3个浓度级异丙醇测试液的回收率为98%~101%。2名分析员分别检测同一样品的6个平行测试液,测定结果的相对标准偏差为0.5%。结论 建
立的方法专属性、准确性、重复性和耐用性良好,可用于异丙醇消毒剂的定量检测。
Objective To establish a gas chromatography for quantitative determination of isopropanol disinfectant. Methods DB-1 gas chromatographic column was used with a size of 30 m (length) × 0.53 mm (inner diameter) × 3.00 µm (film thickness). The temperature programmed mode was adopted. Nitrogen was used as carrier gas with a constant flow rate of 5 ml/min; the temperatures of inlet and detector were 200 and 275 ℃, respectively. Split sampling with sample size of 1 µl was adopted. The specificity, accuracy, repeatability and durability of the method were verified. Results Isopropanol gas and n-butyl alcohol gas were completely separated with a separation degree of 25.4. The method had good linearity within the scope of investigation and the determination coefficient was 0.999 977. No interference peaks appeared in the diluted n-butyl alcohol chromatogram. The recoveries of isopropanol test solutions at 3 concentrations were between 98% and 101%. When 6 parallel solutions of the same sample were tested separately by 2 analysts, the relative standard deviation of the results was 0.5%. Conclusions The established method has good specificity, accuracy, repeatability and durability, and can be used for quantitative detection of isopropanol disinfectant.