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In-situ fabrication of zeolite imidazole framework@hydroxyapatite composite for dispersive solid-phase extraction of benzodiazepines and their determination with high-performance liquid chromatography-VWD detection
Microchimica Acta ( IF 5.3 ) Pub Date : 2020-09-01 , DOI: 10.1007/s00604-020-04517-y Zi-Ling Li 1 , Zi-Yang Zhang 1 , Teng-Wen Zhao 1 , Chun-Yan Meng 1 , Qian-Ying Zhang 2 , Man-Man Wang 1
Microchimica Acta ( IF 5.3 ) Pub Date : 2020-09-01 , DOI: 10.1007/s00604-020-04517-y Zi-Ling Li 1 , Zi-Yang Zhang 1 , Teng-Wen Zhao 1 , Chun-Yan Meng 1 , Qian-Ying Zhang 2 , Man-Man Wang 1
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A novel zeolite imidazole framework@hydroxyapatite composite (ZIF-8@HAP) was constructed via in-situ growth and developed for efficient dispersive solid-phase extraction (DSPE) of three benzodiazepines from urine samples. The prepared composite was characterized by scanning electron microscopy, energy-dispersive spectrometer, Fourier-transform infrared spectrometry, X-ray diffractometry, zeta potential analyzer, and nitrogen adsorption-desorption experiment. Characterization results showed typical dodecahedron ZIF-8 crystals that were uniformly located on the surface of rod-like HAP. The combination of ZIF-8 and HAP made the surface area significantly enhanced from 4.68 to 205.44 m2 g−1. Compared with a commercial C18 adsorbent, ZIF-8@HAP exhibited superior removal performance for interfering components from urine and offered better extraction properties for the analytes. The prepared ZIF-8@HAP was applied as an adsorbent in DSPE, and the main experimental parameters, including pH and ionic strength of solution, adsorbent amount, adsorption time, elution solvent, and volume, were investigated. Under optimal conditions, the adsorption for 250 ng mL−1 of each analyte in 4 mL of urine was accomplished within 2 min using 60 mg of adsorbent. The method of ZIF-8@HAP–based DSPE followed by high-performance liquid chromatography gave enhancement factors of 13.3–15.3, linear ranges of 2.5–500 ng mL−1, and limits of detection (S/N = 3) of 0.7–1.4 ng mL−1. The relative recoveries at three spiked levels ranged from 88.7 - 102% with intra-day and inter-day precisions from 3.0 - 10.3% and 2.3 - 12.3%, respectively. These results indicated that the proposed strategy had promising applicability for convenient, rapid, and efficient determination of benzodiazepines in urine samples. Graphical abstract In-situ fabrication of ZIF-8@HAP composite for dispersive solid-phase extraction of benzodiazepines in urine samples. In-situ fabrication of ZIF-8@HAP composite for dispersive solid-phase extraction of benzodiazepines in urine samples.
中文翻译：
用于苯二氮卓类分散固相萃取的沸石咪唑骨架@羟基磷灰石复合物的原位制备及其高效液相色谱-VWD检测
通过原位生长构建了一种新型沸石咪唑骨架@羟基磷灰石复合材料（ZIF-8@HAP），并开发用于从尿样中高效分散固相萃取（DSPE）三种苯二氮卓类化合物。通过扫描电镜、能谱仪、傅里叶变换红外光谱仪、X射线衍射仪、zeta电位分析仪和氮吸附-解吸实验对制备的复合材料进行了表征。表征结果表明，典型的十二面体 ZIF-8 晶体均匀分布在棒状 HAP 表面。ZIF-8 和 HAP 的组合使表面积从 4.68 显着增加到 205.44 m2 g-1。与商用 C18 吸附剂相比，ZIF-8@HAP 对尿液中的干扰成分表现出优异的去除性能，并为分析物提供了更好的提取性能。将制备的ZIF-8@HAP用作DSPE中的吸附剂，考察了溶液的pH和离子强度、吸附剂用量、吸附时间、洗脱溶剂和体积等主要实验参数。在最佳条件下，使用 60 mg 吸附剂在 2 分钟内完成对 4 mL 尿液中每种分析物 250 ng mL-1 的吸附。基于 ZIF-8@HAP 的 DSPE 和高效液相色谱法的增强因子为 13.3-15.3，线性范围为 2.5-500 ng mL-1，检测限 (S/N = 3) 为 0.7 –1.4 ng mL−1。三个加标水平的相对回收率范围为 88.7 - 102%，日内和日间精度为 3.0 - 10。分别为 3% 和 2.3 - 12.3%。这些结果表明，所提出的策略对于方便、快速、有效地测定尿样中的苯二氮卓类具有良好的适用性。图形摘要 原位制造 ZIF-8@HAP 复合材料，用于尿样中苯二氮卓类的分散固相萃取。原位制备 ZIF-8@HAP 复合材料，用于尿样中苯二氮卓类的分散固相萃取。
更新日期：2020-09-01
中文翻译：
用于苯二氮卓类分散固相萃取的沸石咪唑骨架@羟基磷灰石复合物的原位制备及其高效液相色谱-VWD检测
通过原位生长构建了一种新型沸石咪唑骨架@羟基磷灰石复合材料（ZIF-8@HAP），并开发用于从尿样中高效分散固相萃取（DSPE）三种苯二氮卓类化合物。通过扫描电镜、能谱仪、傅里叶变换红外光谱仪、X射线衍射仪、zeta电位分析仪和氮吸附-解吸实验对制备的复合材料进行了表征。表征结果表明，典型的十二面体 ZIF-8 晶体均匀分布在棒状 HAP 表面。ZIF-8 和 HAP 的组合使表面积从 4.68 显着增加到 205.44 m2 g-1。与商用 C18 吸附剂相比，ZIF-8@HAP 对尿液中的干扰成分表现出优异的去除性能，并为分析物提供了更好的提取性能。将制备的ZIF-8@HAP用作DSPE中的吸附剂，考察了溶液的pH和离子强度、吸附剂用量、吸附时间、洗脱溶剂和体积等主要实验参数。在最佳条件下，使用 60 mg 吸附剂在 2 分钟内完成对 4 mL 尿液中每种分析物 250 ng mL-1 的吸附。基于 ZIF-8@HAP 的 DSPE 和高效液相色谱法的增强因子为 13.3-15.3，线性范围为 2.5-500 ng mL-1，检测限 (S/N = 3) 为 0.7 –1.4 ng mL−1。三个加标水平的相对回收率范围为 88.7 - 102%，日内和日间精度为 3.0 - 10。分别为 3% 和 2.3 - 12.3%。这些结果表明，所提出的策略对于方便、快速、有效地测定尿样中的苯二氮卓类具有良好的适用性。图形摘要 原位制造 ZIF-8@HAP 复合材料，用于尿样中苯二氮卓类的分散固相萃取。原位制备 ZIF-8@HAP 复合材料，用于尿样中苯二氮卓类的分散固相萃取。
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