Guizhou Academy of Tobacco Science, Guiyang 550081, China.
Qiandongnan Company of Guizhou Province of CNTC, Kaili 556000, China.
Molecules. 2024 Apr 30;29(9):2068. doi: 10.3390/molecules29092068.
2, 6-diisopropylaniline (2, 6-DIPA) is a crucial non-intentionally organic additive that allows the assessment of the production processes, formulation qualities, and performance variations in biodegradable mulching film. Moreover, its release into the environment may have certain effects on human health. Hence, this study developed simultaneous heating hydrolysis-extraction and amine switchable hydrophilic solvent vortex-assisted homogeneous liquid-liquid microextraction for the gas chromatography-mass spectrometry analysis of the 2, 6-DIPA additive and its corresponding isocyanates in poly(butylene adipate-co-terephthalate) (PBAT) biodegradable agricultural mulching films. The heating hydrolysis-extraction conditions and factors influencing the efficiency of homogeneous liquid-liquid microextraction, such as the type and volume of amine, homogeneous-phase and phase separation transition pH, and extraction time were investigated and optimized. The optimum heating hydrolysis-extraction conditions were found to be a HSO concentration of 2.5 M, heating temperature of 87.8 °C, and hydrolysis-extraction time of 3.0 h. As a switchable hydrophilic solvent, dipropylamine does not require a dispersant. Vortex assistance is helpful to speed up the extraction. Under the optimum experimental conditions, this method exhibits a better linearity (0.01447.200 μg mL with = 0.9986), low limit of detection and quantification (0.0033 μg g and 0.0103 μg g), high extraction recovery (92.5105.4%), desirable intra- and inter-day precision (relative standard deviation less than 4.1% and 4.7%), and high enrichment factor (90.9). Finally, this method was successfully applied to detect the content of the additive 2, 6-DIPA in PBAT biodegradable agricultural mulching films, thus facilitating production process monitoring or safety assessments.
2,6-二异丙基苯胺(2,6-DIPA)是一种重要的非故意有机添加剂,可用于评估可生物降解覆盖膜的生产工艺、配方质量和性能变化。此外,它释放到环境中可能对人类健康产生一定影响。因此,本研究开发了同时加热水解提取和胺切换亲水溶剂涡旋辅助均相液相微萃取,用于气相色谱-质谱分析聚(丁二酸丁二醇酯-己二酸酯)(PBAT)可生物降解农用覆盖膜中的 2,6-DIPA 添加剂及其相应异氰酸酯。优化了加热水解提取条件和影响均相液相微萃取效率的因素,如胺的类型和体积、均相相和相分离过渡 pH 值以及萃取时间。发现最佳加热水解提取条件为 HSO 浓度为 2.5 M,加热温度为 87.8°C,水解提取时间为 3.0 h。作为一种可切换亲水溶剂,二丙胺不需要分散剂。涡旋辅助有助于加快提取速度。在最佳实验条件下,该方法具有较好的线性范围(0.01447.200 μg mL,r=0.9986)、较低的检测限和定量限(0.0033 μg g 和 0.0103 μg g)、较高的萃取回收率(92.5105.4%)、良好的日内和日间精密度(相对标准偏差小于 4.1%和 4.7%)和高富集因子(90.9)。最后,该方法成功应用于检测 PBAT 可生物降解农用覆盖膜中添加剂 2,6-DIPA 的含量,从而有利于生产过程监测或安全评估。