UPLC-MS/MS法测定尿液中反—反式粘糠酸

崔师伟; 周晓滢; 邢彩虹; 闫慧芳

doi:10.13421/j.cnki.hjwsxzz.2022.12.010

UPLC-MS/MS法测定尿液中反—反式粘糠酸

Determination of trans, trans-muconic acid in urine by UPLC-MS/MS

摘要

摘要:
目的建立尿液中反—反式粘糠酸的超高效液相色谱串联质谱测定方法。
方法尿液加入同位素标记的反—反式粘糠酸内标，采用强阴离子固相萃取柱进行净化，经Shield RP18色谱柱分离，三重四级杆质谱检测，内标法定量。
结果反—反式粘糠酸的线性范围为20.0~1 000.0 μg/L，相关系数为0.999 7；方法的检出限和定量限分别为1.10 μg/L和3.30 μg/L；加标浓度为50.0、200.0、800.0 μg/L时，方法的加标回收率为98.3%~101%；批内精密度（RSD）为0.88%~2.79%，批间精密度（RSD）为3.38%~5.63%。
结论本方法适用于尿液中反—反式粘糠酸的测定。

Abstract:
Objective To establish a method for determination of trans, trans-muconic acid in urine by UPLC-MS/MS.
Methods Trans, trans-muconic acid which was labeled by the isotope was added to the urine samples. Then the samples were purified by solid phase extraction column and separated by Shield RP18 chromatographic column, and detected by the triple quadrupole mass spectrometry. The contents of trans, trans-muconic acid were quantified by the internal standard method.
Results The linear range of trans, trans-muconic acid was 20.0-1 000.0 μg/L, with a correlation coefficient of 0.9997. The detection limit and the quantification limit were 1.10 μg/L and 3.30 μg/L, respectively. The spiked recovery rate of this method was 98.3%-101% at the spiked concentrations of 50.0, 200.0, and 800.0 μg/L.The within-run and between-run relative standard deviation(RSD) were 0.88%-2.79% and 3.38%-5.63%, respectively.
Conclusion This method is suitable for the determination of trans, trans-muconic acid in urine.

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