基于聚苯乙烯纳米纤维的固相萃取结合液质联用技术同时检测人尿液中的4种非典型抗精神病药物  

Determination of four atypical antipsychotics in human urine by UPLC-MS/MS with polystyrene nanofibers as solid-phase extraction sorbent

作　　者：范理菊 安静[1] 董占军[1] FAN Li-ju;AN Jing;DONG Zhan-jun(Pharmaceutical Department,Hebei General Hospital,Shijiazhuang 050051,Hebei Province,China)

机构地区：[1]河北省人民医院药学部,河北石家庄050051

出　　处：《中国临床药理学杂志》2024年第12期1818-1821,共4页The Chinese Journal of Clinical Pharmacology

摘　　要：目的 开发一种基于聚苯乙烯纳米纤维的固相萃取结合超高效液相色谱串联质谱法测定人尿液中氨磺必利、奥氮平、利培酮、帕利哌酮4种非典型抗精神病药物。方法 用静电纺丝技术制备聚苯乙烯纳米纤维,并以聚苯乙烯纳米纤维为吸附剂制备固相萃取小柱萃取人尿液中的4种非典型抗精神病药物;色谱柱采用Waters XBridge BEH C18,流动相为0.1%甲酸水溶液(A)-乙腈(B),梯度洗脱,流速:0.25 mL·min^(-1),柱温:40℃,进样量:3μL。考察该方法的专属性、标准曲线、定量下限、精密度、准确度、提取回收率、基质效应和稳定性。结果 4种分析物的线性范围均为1~100 ng·mL^(-1),相关系数均大于0.996。定量下限为1 ng·mL^(-1),检测限为0.01~0.10 ng·mL^(-1)。4种分析物的批内、批间相对标准偏差(RSD)范围为2.34%~14.48%,提取回收率均大于75.75%,基质效应基质效应在85.00%~115.00%。各样品在自动进样器中放置24 h稳定性RSD为2.19%~12.06%;冻融3次稳定性RSD为3.65%~13.81%。结论 本法灵敏度高,适用于尿液样本中微量分析物的提取和测定,为抗精神病药物检测提供了可靠的分析手段。Objective To develop a novel micro-extraction procedure based on polystyrene nanofibers as solid-phase extraction sorbent to extract four atypical antipsychotics including amisulpride,olanzapine,risperidone,paliperidone from human urine samples.Methods Polystyrene nanofibers were prepared by electrostatic spinning technique,and four atypical antipsychotics in human urine were extracted by a solid phase extraction column using polystyrene nanofibers as sorbent.The detection was performed on Waters XBridge BEH C18 with the mobile phase of 0.1 % formic acid aqueous solution(A)-acetonitrile(B) by a gradient elution at 0.25 mL·min^(-1) flow rate.The temperature of column was 40 ℃ and the injection volume was 3 μL.The method's selectivity,standard curves,quantification limit,precision,accuracy,extraction recovery,matrix effect,and stability were assessed.Results The linear ranges of the four analytes were found to be 1-100 ng·mL^(-1),with correlation coefficients all exceeding 0.996.The lower limit of quantification was 1 ng · mL^(-1),and the limit of quantitation ranged from 0.01-0.10 ng · mL^(-1).The intra-day and inter-day RSDs for the four analytes ranged from2.34%-14.48%,with extraction recoveries all exceeding 75.75%.The matrix effect falls within the range of85.00%-115.00%.The stability of samples placed in the autosampler for 24 hours exhibited RSDs ranging from2.19%-12.06%,while the stability after three freeze-thaw cycles ranged from 3.65%-13.81%.Conclusion This method is sensitive and suitable for the determination of target analytes in complex matrices,and provides a reliable analytical tool for the detection of atypical antipsychotics.

关 键 词：聚苯乙烯纳米纤维 固相萃取 超高效液相色谱串联质谱 抗精神病药物 尿液样本 

分 类 号：R97[医药卫生—药品]