Xie Li, Shen Jingyi, Shu Qing, Ge Weihong, Yang Xiuhua, Hussian Ahad, Kang Xuejun
College of Animal Science and Technology, Jinling Institute of Technology Nanjing 210038 China.
Department of Pharmacy, Nanjing Drum Tower Hospital Nanjing China.
RSC Adv. 2025 May 8;15(19):15017-15028. doi: 10.1039/d5ra00930h. eCollection 2025 May 6.
Methotrexate (MTX) is a drug that has long been used in high doses as an anti-cancer drug and lately in low doses as a treatment for autoimmune diseases. It is necessary to be determined in various matrices because the drug has a narrow therapeutic range and a high persistence in the environment. Since MTX and its polyglutamate metabolites (MTXPGs) have strong polarity and the potential to be converted during sample processing, rapid and efficient extraction of these targets has provided technical challenges for development of analytical methods for them. A new Pd(ii)/polyethyleneimine (PEI)/polystyrene (PS) nanofibre was prepared and characterized by X-ray diffraction, FTIR spectroscopy, thermal analysis, scanning electron microscopy and transmission electron microscopy, The nanofibre was applied as a sorbent to extract MTX and MTXPGs in whole blood and MTX in urine and water. The extracted analytes were then desorbed by a water solution containing 10% methanol and 20% ammonium hydroxide (v/v) and eventually quantified by high performance liquid chromatography. The peak area of the target substances in the extraction solution and its concentration were linear in the range of 20.0 (∼37.8 to 1000 ng/mL); intraday and interday RSD were 4.6-6.4% and 5.7-14.6%, respectively. The detection limit of this method was 6.0-11.3 ng/mL. The results showed that the method can be used for the determination of MTX and MTXPGs in human whole blood and MTX in urine/water samples.
甲氨蝶呤（MTX）是一种长期以来高剂量用作抗癌药物、近来低剂量用于治疗自身免疫性疾病的药物。由于该药物治疗范围窄且在环境中持久性高，因此有必要在各种基质中对其进行测定。由于MTX及其聚谷氨酸代谢物（MTXPGs）具有很强的极性且在样品处理过程中可能发生转化，快速高效地提取这些目标物给其分析方法的开发带来了技术挑战。制备了一种新型的钯（II）/聚乙烯亚胺（PEI）/聚苯乙烯（PS）纳米纤维，并通过X射线衍射、傅里叶变换红外光谱、热分析、扫描电子显微镜和透射电子显微镜对其进行了表征。该纳米纤维用作吸附剂，用于提取全血中的MTX和MTXPGs以及尿液和水中的MTX。然后用含有10%甲醇和20%氢氧化铵（v/v）的水溶液对提取的分析物进行解吸，最终通过高效液相色谱进行定量。提取溶液中目标物质的峰面积与其浓度在20.0（约37.8至1000 ng/mL）范围内呈线性关系；日内和日间相对标准偏差分别为4.6 - 6.4%和5.7 - 14.6%。该方法的检测限为6.0 - 11.3 ng/mL。结果表明，该方法可用于测定人全血中的MTX和MTXPGs以及尿液/水样中的MTX。
