超高效液相色谱-三重四极杆质谱法测定血浆和尿液中马桑亭和马桑宁

建立了超高效液相色谱-三重四极杆质谱联用技术测定血浆和尿液中马桑中毒标志物马桑亭和马桑宁的方法。血浆和尿液样品经固相支持液液萃取法提取净化后,溶于15%(v/v)甲醇水溶液中,以Cortecs C₁₈色谱柱(100 mm×2.1 mm, 1.6μm)作为分析柱进行分离,电喷雾负离子多反应监测(MRM)模式下检测,以氟苯尼考作为内标物,基质工作曲线内标法定量。血浆和尿液中马桑亭和马桑宁的平均加标回收率为86.2%～110%,相对标准偏差为5.1%～14.6%(n=6),血浆中马桑亭和马桑宁的检出限(S/N=3)分别为0.01μg/L和0.1μg/L,尿液中马桑亭和马桑宁的检出限分别为0.03μg/L和0.3μg/L。本法简单、灵敏、准确,可用于血浆和尿液中马桑亭和马桑宁的中毒检测。

Determination of coriatin and corianin in plasma and urine using ultra-performance liquid chromatography-triple quadrupole mass spectrometry

An ultra-performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-MS/MS) method has been developed for the determination of coriatin and corianin in plasma and urine, which are the biomarkers of poisoning caused by Coriaria sinica Maxim. Plasma and urine samples were extracted and purified using a solid supported liquid/liquid extraction method. Chromatographic separation was performed on a Cortecs C₁₈ column (100 mm×2.1 mm, 1.6 μm) using a gradient elution of methanol and water. Coriatin and corianin were detected using negative electrospray ionization tandem mass spectrometry in multiple reaction monitoring (MRM) mode and quantified via a matrix working standard curve internal standard method; florfenicol was used as the internal standard. The assay was linear in the calibration range of 0.03-5.0 μg/L for coriatin and 0.3-50 μg/L for corianin in plasma, and 0.1-10 μg/L and 1-100 μg/L for coriatin and corianin in urine, respectively. The average recoveries were 86.2%-110% for coriatin and corianin in plasma and urine with relative standard deviations of 5.1%-14.6% (n=6). The limits of detection (S/N=3) for coriatin and corianin were 0.01 μg/L and 0.1 μg/L in plasma, and 0.03 μg/L and 0.3 μg/L in urine, respectively. The method is simple, sensitive and accurate for the determination of coriatin and corianin in plasma and urine for toxicological purposes.