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建立一种测定人体尿液赭曲霉毒素A(OTA)含量的分子印迹聚合物固相萃取柱净化、高效液相色谱-荧光检测(HPLC-FLD)方法。尿液样品在北京地区随机收集,用0.1 mol·L-1 HCl溶液调至pH 2.5,经分子印迹聚合物固相萃取柱净化后,HPLC-FLD检测其所含赭曲霉毒素A的含量,液相色谱-质谱法(LC-MS/MS)确证阳性样品。赭曲霉毒素A在0.75~250 ng·mL-1内线性关系良好。OTA在3个加样水平的回收率为90.6%~101.9%,RSD为0.1%~1.6%。65份志愿者尿液共检测出5份阳性样品,OTA最大含量为0.091 ng·mL-1。本文首次将分子印迹聚合物固相萃取柱应用于净化和富集人体尿液中的OTA,方法简单、快速、可靠,适用于人体尿液中OTA的检测。
To establish a HPLC-FLD method for the determination of ochratoxin A (OTA) in human urine by molecularly imprinted polymer SPE cartridges and high performance liquid chromatography-fluorescence detection (HPLC-FLD). Urine samples were randomly collected in Beijing area and adjusted to pH 2.5 with 0.1 mol·L-1 HCl solution. After purification by molecularly imprinted polymer SPE column, the content of ochratoxin A contained in the urine sample was detected by HPLC- Positive samples were confirmed by LC-MS / MS. Ochratoxin A showed good linearity within 0.75-250 ng · mL-1. The recoveries of OTA at three loading levels ranged from 90.6% to 101.9% with RSDs ranging from 0.1% to 1.6%. A total of 5 positive samples were detected in urine of 65 volunteers. The maximum content of OTA was 0.091 ng · mL-1. This paper, for the first time, uses molecularly imprinted polymer SPE columns to purify and enrich OTA in human urine. The method is simple, rapid and reliable and is suitable for the detection of OTA in human urine.