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Dispersive solid-phase extraction based on zirconium metal-organic framework coupled with gas chromatography-mass spectrometry for determining sugar phosphates in biological samples
Analytica Chimica Acta ( IF 5.7 ) Pub Date : 2024-06-25 , DOI: 10.1016/j.aca.2024.342908
Yuyan Hu , Boxue Wu , Ying-Shu Tang , Yi Wu , Li-Yan Liu

Sugar phosphates (SPx) play important role in the metabolism of the organism. SPx such as glycerate 3-phosphate, fructose 6-phosphate and glucose 6-phosphate in biological samples have the poor stability, similar structure and low abundance, which make their separation and detection more challenging. UiO-66-NH and ZrO coated SiO(SBA-15) hard-core–shell adsorbents (UiO-66-NH@SBA-15 and ZrO@SBA-15) were synthesized, which were further used for dispersive solid-phase extraction for enriching the SPx in biological samples. The protocol was developed by UiO-66-NH@SBA-15 and ZrO@SBA-15 coupled with gas chromatography-mass spectrometry for the detection of trace SPx. The univariate experiment and response surface methodology were used to optimize the adsorption and desorption conditions. The adsorbents showed excellent adsorption capacity and specificity towards SPx, which were proved by adsorption and selective experiments. Under the optimized conditions, there were good linearity within the range of 5.0–5000.0 ng mL, low limits of detection (0.001–1.0 ng mL), low limits of quantification (0.005–5.0 ng mL) and good precision (relative standard deviation less than 14.7 % for intra-day and inter-day). The satisfactory recoveries (89.1–113.8 %) and precision (0.5–14.6 %) were obtained when the sorbents were used to extract SPx from serum, saliva and cell samples. Moreover, UiO-66-NH@SBA-15 was applied to the quantitative analysis of SPx from gastric cancer patients, because of a higher adsorption capacity (169.5–196.1 mg g). UiO-66-NH@SBA-15 showed great potential in the extraction of SPx in biological samples, which was beneficial to find out the metabolic change of SPx and explain the pathogenesis of the disease.

中文翻译:


基于锆金属有机骨架的分散固相萃取联合气相色谱-质谱法测定生物样品中的磷酸糖



糖磷酸盐(SPx)在生物体的新陈代谢中发挥着重要作用。生物样品中的3-磷酸甘油酯、6-磷酸果糖、6-磷酸葡萄糖等SPx稳定性较差、结构相似、丰度较低,这使得它们的分离和检测更具挑战性。合成了 UiO-66-NH 和 ZrO 包覆 SiO(SBA-15) 硬核壳吸附剂(UiO-66-NH@SBA-15 和 ZrO@SBA-15),并进一步用于分散固相萃取用于富集生物样品中的 SPx。该协议是由 UiO-66-NH@SBA-15 和 ZrO@SBA-15 与气相色谱-质谱联用开发的,用于检测痕量 SPx。采用单变量实验和响应面法来优化吸附和解吸条件。吸附和选择性实验证明该吸附剂对SPx表现出优异的吸附能力和特异性。在优化条件下,在5.0~5000.0 ng mL范围内线性良好,检出限低(0.001~1.0 ng mL),定量限低(0.005~5.0 ng mL),精密度好(相对标准偏差较小)。日内和日间的比率高于 14.7%)。当使用吸附剂从血清、唾液和细胞样品中提取 SPx 时,获得了令人满意的回收率 (89.1–113.8 %) 和精密度 (0.5–14.6 %)。此外,UiO-66-NH@SBA-15 由于具有较高的吸附容量(169.5–196.1 mg g)而被应用于胃癌患者 SPx 的定量分析。 UiO-66-NH@SBA-15在生物样品中SPx的提取方面显示出巨大的潜力,有利于找出SPx的代谢变化并解释疾病的发病机制。
更新日期:2024-06-25
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