高效液相色谱法检测防腐橡胶木中的碘代丙炔基丁基氨基甲酸酯

橡胶木中淀粉含量远高于其他树种,易发霉、蓝变。碘代丙炔基丁基氨基甲酸酯（3-iodo-2-propynyl butyl carbamate,IPBC）绿色环保,对霉菌、蓝变菌有特效,尤其适用于橡胶木保护。目前橡胶木中IPBC分析方法的研究报道较少,其防腐处理材的质量监督尚缺乏有效手段。为了准确分析防腐橡胶木中的IPBC,建立了一种高效液相色谱（high-performance liquid chromatography,HPLC）方法,检验了该方法的检出限、加标回收率等性能,并比较了不同提取方法、提取溶剂、木粉粒径等因素对防腐橡胶木中IPBC提取效果的影响。建立的HPLC方法使用C18反相色谱柱,乙腈-水（55︰45,V/V）为流动相,流速1.0 mL/min,检测波长204 nm,IPBC保留时间约6.45 min。在2~80 mg/L浓度范围内,线性关系良好,相关系数0.9998;检出限0.2 mg/L,平均加标回收率99.61%。超声法提取的效果显著优于索氏抽提器法;以甲醇或甲醇-水（9︰1, V/V）混合液为溶剂超声提取的效果较好,乙酸乙酯和石油醚不适于提取木材中的IPBC。以甲醇-水（9︰1, V/V）混合液为溶剂制备样品可改善色谱峰形,有助于提高分析方法的准确性。木粉粒径差异对IPBC超声提取的影响较小。高温条件会导致IPBC降解,严重影响分析结果准确性,因此在整个分析过程中应避免高温条件。本方法检出限低、重现性好,准确性高,适于分析防腐木材中微量的IPBC。

Determination of Iodopropynyl Butyl Carbamate in Treated Rubber Wood by High Performance Liquid Chromatography

Rubber wood is known to be very susceptible to mold and sap stain fungi attacks because of its extraordinary high starch content. 3-iodo-2-propynyl butyl carbamate (IPBC) is suitable for rubber wood preservation as it is highly effective in mold and sap stain fungi, and environmentally friendly. However, few studies on the quantitation methods of IPBC in treated rubber wood have been reported. To determine IPBC in treated rubber wood accurately, a high-performance liquid chromatography (HPLC) method was developed, and the optimization of extracting IPBC from rubber wood was conducted by comparing the effects of different extraction methods, solvents, and particle sizes of wood powder. The HPLC conditions were as follows: C18 reversed-phase column, acetonitrile-water (55︰45, V/V) as mobile phase, flow rate 1.0 mL/min, detection wavelength 204 nm, the retention time of IPBC about 6.45 min. There was a good linear correlation between the mass concentration of IPBC and the peak area with a correlation coefficient of 0.9998 in the range of 2~80 mg/L. The limit of detection (LOD) was 0.2 mg/L, and the average recovery of spiked samples was 99.61%. The comparison of extraction methods showed that ultrasonic extraction was significantly better than the Soxhlet extraction. Methanol or methanol-water (9︰1, V/V) mixed solution was the best solvent to extract IPBC from wood, but ethyl acetate and petroleum ether were not suitable for extracting. Using methanol-water (9︰1, V/V) as the solvent could eliminate the leading peak, which was helpful to improve the accuracy of the analytical method. The difference in wood powder particle size had little effect on the analysis results of IPBC extracted by ultrasonic. The enormous degradation of IPBC due to high temperature greatly affected the analysis results, therefore, high-temperature conditions should be avoided during the analysis process. With the advantages of low detective limit, good reproducibility, and high accuracy, the developed method may have great potential for the analysis of IPBC in preservative woods.