IPBC高效液相色谱分析方法及处理材抗流失性能

韩利平; 王卿平; 张景朋; 蒋明亮; 曹金珍

doi:10.12171/j.1000-1522.20210049

摘要:

目的为了探究3-碘-2-丙炔基−丁基氨基甲酸酯（IPBC）制剂的抗流失性能，本研究建立IPBC含量的高效液相色谱（HPLC）分析方法，并对各处理材流失液中的IPBC含量进行测定，旨在确定IPBC制剂的抗流失性能。

方法采用紫外检测器及C₁₈色谱柱（150 mm × 4.6 mm（内径），5 μm），通过对检测波长、流动相组成及配比、柱温及流动相流速等色谱条件进行优化，确定分析IPBC的色谱条件，采用外标法对IPBC标准溶液进行检测，进行标准曲线相关系数、精密度、准确度等分析；参照国家标准GB/T 29905—2013《木材防腐剂流失率试验方法》进行流失试验，用所建立的分析方法测定各处理材中IPBC的流失率。

结果 HPLC检测IPBC含量的色谱条件为：乙腈–水（体积比为60∶40）为流动相，流速为1.0 mL/min，紫外检测波长为200 nm；IPBC标准溶液在5 ~ 80 mg/L浓度范围内，HPLC标准曲线的相关系数为0.999 4，标准偏差0.05%，变异系数0.50%，样品的添加回收率为99.5% ~ 100.4%；马尾松和辐射松处理材中IPBC的流失率随着IPBC浓度的增加而降低，马尾松的流失率为0.11% ~ 1.99%，辐射松的流失率为0.10% ~ 0.48%，毛竹处理材中IPBC的流失率随着IPBC浓度的增加而增加，流失率为3.11% ~ 7.08%；IPBC制剂处理材的平均流失率高于IPBC/PPZ-TEB复合制剂处理材的平均流失率；微乳D制剂处理材IPBC的流失率高于IPBC乙醇溶液处理材的流失率；经过木蜡油表面涂饰的IPBC制剂处理材的流失率低于未涂饰的IPBC制剂处理材的流失率。

结论采用HPLC测定IPBC的含量，标准曲线相关系数好，精密度和准确度高，可用于IPBC的含量分析；IPBC制剂的抗流失性能较好，其在马尾松、辐射松、毛竹处理材中的流失率均低于7.1%；通过与其他成分复合或木蜡油进行表面涂饰可以提高IPBC制剂的抗流失性能。

Abstract:

Objective In order to explore the leachability of iodopropynyl butylcarbamate (IPBC) formulations, an analytical method of IPBC by high performance liquid chromatography (HPLC) was established and used for the determination of IPBC leaching rate of treated wood and bamboo, aiming to determine an analytical method of IPBC by HPLC and the leachability of IPBC.

Method UV detector and C₁₈ column (150 mm × 4.6 mm (inner diameter), 5 μm) were used for detection. The chromatographic conditions, such as detection wavelength, mobile phase composition and ratio, column temperature and mobile phase flow rate were investigated and discussed, so as to optimize the chromatographic conditions suitable for the analysis of IPBC. The IPBC standard solution was detected by external standard method. The standard curve, precision and accuracy were evaluated. The leaching procedure was adopted according to the Chinese standard method. The IPBC leachability rate was tested in treated wood and bamboo by the established analytical method.

Result The chromatographic conditions for the determination of IPBC content by HPLC were as follows: flow phase acetonitrile-water (60∶40), flow rate 1.0 mL/min, UV detection wavelength 200 nm. There was a good linear relationship between IPBC concentration and chromatographic peak area in the range of 5−80 mg/L for IPBC standard solution. The correlation coefficient was r = 0.999 4. The standard deviation and coefficient of variation were 0.05% and 0.50%, respectively. The recovery rates were 99.5%−100.4%. The leaching rate of IPBC in Masson pine and radiation pine decreased with the increase of IPBC concentration, the leaching rate of Masson pine ranged from 0.11% to 1.99%, the leaching rate of radiation pine ranged from 0.10% to 0.48%. In bamboo, the leaching rate of IPBC increased with the increase of IPBC concentration, with the leaching rate ranged from 3.11% to 7.08%. The average leaching rate of IPBC treated bamboo was higher than IPBC/PPZ-TEB. The leaching rate of IPBC micro emulsion in treated wood was higher than that dissolved with ethanol. The leaching rate of IPBC with surface coating of hard wax oil in treated wood was lower than that without surface coating.

Conclusion The determination method of IPBC content by HPLC with good correlation, high precision and recovery rate could be used for the analysis of IPBC content. The leaching rates of IPBC treated masson pine, radiant pine and bamboo were very low as less than 7.1%. The leaching rate of IPBC could be decreased by mixing with other agents or surface coating with hard wax oil.

IPBC高效液相色谱分析方法及处理材抗流失性能

Analytical method of IPBC by HPLC and leachability in treated wood and bamboo