Conjugated microporous polymers (CMPs) with uniform morphology have shown fascinating application in the separation science. In this study, metal-free Knoevenagel condensation was adopted to prepare spherical sp² carbon-conjugated microporous polymers, which used tetrakis(4-formylphenyl)methane and 1,4-phenylenediacetonitrile as monomers. Due to the remarkable extraction capability for carbamate pesticides (CPs), the as-synthesized CMPs were fabricated as the coating for solid-phase microextraction (SPME). After optimized SPME parameters (adsorption time, salt concentration, sample pH, adsorption temperature, desorption time, desorption solvent and desorption volume), ten CPs in water samples were quantified by ultrahigh performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). Linearity in the range 0.005–100 ng mL⁻¹ with low detection limits of 0.00060–0.017 ng mL⁻¹ was obtained. The intra-day and inter-day precisions expressed as relative standard deviations were 1.5–8.1% and 1.1–8.0%, respectively. Fiber-to-fiber reproducibility was below 7.3%. The CMPs-SPME-UPLC-MS/MS method was applied to detect trace CPs in real water samples with relative recoveries from 91.8% to 108%.

具有均匀形态的共轭微孔聚合物（CMP）在分离科学中显示出令人着迷的应用。在这项研究中，采用无金属的Knoevenagel缩合制备球形sp ²碳共轭微孔聚合物，它使用四（4-甲酰基苯基）甲烷和1,4-苯二乙腈作为单体。由于对氨基甲酸酯类农药（CPs）具有出色的提取能力，因此将合成后的CMPs制成了固相微萃取（SPME）的涂层。经过优化SPME参数（吸附时间，盐浓度，样品pH，吸附温度，脱附时间，脱附溶剂和脱附体积）后，通过超高效液相色谱串联质谱（UPLC-MS / MS）对水中的10个CP进行了定量。线性范围为0.005–100 ng mL ^-1，检测下限为0.00060–0.017 ng mL ^-1获得了。以相对标准偏差表示的日内和日间精度分别为1.5–8.1％和1.1–8.0％。光纤到光纤的重复性低于7.3％。CMPs-SPME-UPLC-MS / MS方法用于检测真实水样中的痕量CP，相对回收率从91.8％至108％。