Abstract A new magnetic field-assisted solid-phase extraction (MFA-SPE) procedure was developed by merging the features of magnetic solid-phase extraction and magnetic in-tube solid-phase microextraction. The MFA-SPE method was coupled with HPLC-UV and applied for the separation and determination of anti-HIV drugs in biological fluids. Magnetic Fe3O4@PANI nanocomposite with core/shell structure was synthesized and used as the extraction phase. It was characterized by FT-IR, SEM, and EDX techniques. Type and volume of eluting solvent, magnetic field intensity, and pH, ionic strength, and volume of the sample solution were studied as the influential parameters. The calibration graphs were linear in the range of 1–5000 ng/mL, with linear regression coefficients greater than 0.99. The LOD was calculated 0.1 ng/mL for both analytes. For six replicated analyses of sample solutions containing 500 ng/mL of zidovudine and lamivudine, the intra-day and inter-day RSDs were calculated 4.1–8.8% and 3.2–13.7%, respectively. Under the optimized conditions, the mean recoveries (n = 3) of the analytes in spiked urine samples were obtained 85.1–103.7%. The maximum cartridge adsorption capacity of the Fe3O4/PANI sorbent was obtained 3.9 ± 0.34 and 1.9 ± 0.25 µg/g for zidovudine and lamivudine, respectively. The method applicability in complex matrices was evaluated by the determination of zidovudine and lamivudine in urine samples and commercial pharmaceuticals. Exposing the magnetic sorbent to the external magnetic field led to remarkable higher extraction efficiencies for the selected drugs. Graphical Abstract

中文翻译：

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Fe3O4@PANI核/壳纳米复合材料的磁场辅助固相萃取核苷类药物

摘要 结合磁性固相萃取和磁性管内固相微萃取的特点，开发了一种新的磁场辅助固相萃取（MFA-SPE）方法。MFA-SPE方法与HPLC-UV联用，应用于生物体液中抗HIV药物的分离测定。合成了具有核/壳结构的磁性 Fe3O4@PANI 纳米复合材料并用作萃取相。它通过 FT-IR、SEM 和 EDX 技术进行了表征。洗脱溶剂的类型和体积、磁场强度、pH、离子强度和样品溶液的体积作为影响参数进行了研究。校准图在 1–5000 ng/mL 范围内呈线性，线性回归系数大于 0.99。两种分析物的 LOD 计算值为 0.1 ng/mL。对于含有 500 ng/mL 齐多夫定和拉米夫定的样品溶液的六次重复分析，计算得出的日内和日间 RSD 分别为 4.1-8.8% 和 3.2-13.7%。在优化条件下，加标尿样中分析物的平均回收率 (n = 3) 为 85.1-103.7%。对于齐多夫定和拉米夫定，Fe3O4/PANI 吸附剂的最大滤芯吸附容量分别为 3.9 ± 0.34 和 1.9 ± 0.25 µg/g。通过测定尿样和商业药品中的齐多夫定和拉米夫定来评估该方法在复杂基质中的适用性。将磁性吸附剂暴露于外部磁场可显着提高所选药物的提取效率。图形概要 计算得出的日内和日间 RSD 分别为 4.1-8.8% 和 3.2-13.7%。在优化条件下，加标尿样中分析物的平均回收率 (n = 3) 为 85.1-103.7%。对于齐多夫定和拉米夫定，Fe3O4/PANI 吸附剂的最大滤芯吸附容量分别为 3.9 ± 0.34 和 1.9 ± 0.25 µg/g。通过测定尿样和商业药品中的齐多夫定和拉米夫定来评估该方法在复杂基质中的适用性。将磁性吸附剂暴露于外部磁场可显着提高所选药物的提取效率。图形概要 计算得出的日内和日间 RSD 分别为 4.1-8.8% 和 3.2-13.7%。在优化条件下，加标尿样中分析物的平均回收率 (n = 3) 为 85.1-103.7%。对于齐多夫定和拉米夫定，Fe3O4/PANI 吸附剂的最大滤芯吸附容量分别为 3.9 ± 0.34 和 1.9 ± 0.25 µg/g。通过测定尿样和商业药品中的齐多夫定和拉米夫定来评估该方法在复杂基质中的适用性。将磁性吸附剂暴露于外部磁场可显着提高所选药物的提取效率。图形概要 加标尿液样品中分析物的平均回收率 (n = 3) 为 85.1–103.7%。对于齐多夫定和拉米夫定，Fe3O4/PANI 吸附剂的最大滤芯吸附容量分别为 3.9 ± 0.34 和 1.9 ± 0.25 µg/g。通过测定尿样和商业药品中的齐多夫定和拉米夫定来评估该方法在复杂基质中的适用性。将磁性吸附剂暴露于外部磁场可显着提高所选药物的提取效率。图形概要 加标尿液样品中分析物的平均回收率 (n = 3) 为 85.1–103.7%。对于齐多夫定和拉米夫定，Fe3O4/PANI 吸附剂的最大滤芯吸附容量分别为 3.9 ± 0.34 和 1.9 ± 0.25 µg/g。通过测定尿样和商业药品中的齐多夫定和拉米夫定来评估该方法在复杂基质中的适用性。将磁性吸附剂暴露于外部磁场可显着提高所选药物的提取效率。图形概要 通过测定尿样和商业药品中的齐多夫定和拉米夫定来评估该方法在复杂基质中的适用性。将磁性吸附剂暴露于外部磁场可显着提高所选药物的提取效率。图形概要 通过测定尿样和商业药品中的齐多夫定和拉米夫定来评估该方法在复杂基质中的适用性。将磁性吸附剂暴露于外部磁场可显着提高所选药物的提取效率。图形概要