Zhang Xiuyao, Cai Xinxin, Zhang Xiaoyi, Li Ruifen
Wenzhou Municipal Center for Disease Control and Prevention, Wenzhou 325001, China.
Se Pu. 2019 Feb 8;37(2):149-154. doi: 10.3724/SP.J.1123.2018.09025.
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 C 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% (=6). The limits of detection (=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.
已开发出一种超高效液相色谱 - 三重四极杆质谱法(UPLC-MS/MS)用于测定血浆和尿液中的马桑亭和马桑宁,它们是马桑中毒的生物标志物。血浆和尿液样品采用固相支持液 - 液萃取法进行提取和净化。使用甲醇和水的梯度洗脱在Cortecs C柱(100 mm×2.1 mm,1.6 μm)上进行色谱分离。马桑亭和马桑宁采用负电喷雾电离串联质谱在多反应监测(MRM)模式下进行检测,并通过基质工作标准曲线内标法进行定量;氟苯尼考用作内标。该测定法在血浆中马桑亭的校准范围为0.03 - 5.0 μg/L、马桑宁的校准范围为0.3 - 50 μg/L时呈线性,在尿液中马桑亭的校准范围为0.1 - 10 μg/L、马桑宁的校准范围为1 - 100 μg/L时呈线性。血浆和尿液中马桑亭和马桑宁的平均回收率为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测限(n = 3)分别为0.01 μg/L和0.1 μg/L,尿液中分别为0.03 μg/L和0.3 μg/L。该方法用于毒理学目的测定血浆和尿液中的马桑亭和马桑宁简单、灵敏且准确。