超高效液相色谱-串联质谱法测定沉积物中54种PPCPsOA

A method was established for the determination of 54 pharmaceuticals and personal care products(PPCPs)in sediments by ultra-high performance liquid chromatography-tandem mass spec-trometry(UPLC-MS/MS)coupled with ultrasonic extraction and QuEChERS purification.Samples were treated with Na2EDTA-McIlvaine buffer and acetonitrile containing 0.5％formic acid.Followed by vortex mixing,ultrasonic extraction and centrifugation,the supernatant was purified by a sorbent mixture of anhydrous magnesium sulfate,N-propylethylenediamine(PSA),octadecyl bonded silica gel(C18)and graphitized carbon black(GCB).Chromatographic separation was achieved on an AC-QUITY UPLC BEH C18 column(100 mm×2.1 mm,1.7 μm)with a mobile phase consisting of metha-nol and 5 mmol/L ammonium formate containing 0.1％formic acid.Mass spectrometric detection was performed in multiple reaction monitoring(MRM)mode,with quantification using the internal stan-dard method.The results showed that 54 PPCPs had good linear relationships within their respective mass concentration ranges,with correlation coefficients(r)ranging from 0.997 9 to 0.999 9.The limits of detection(LODs)and limits of quantification(LOQs)ranged from 0.024 to 0.787 μg/kg and 0.094 to 3.145 μg/kg,respectively.Recoveries of the 54 PPCPs at 2.0,5.0,and 10 μg/kg spiked levels were in the range of 74.5％-114％,and the relative standard deviations(RSDs)for par-allel groups were in the range of 2.7％-12％.11 samples of riverine and coastal sediments were ana-lyzed using the established method and 4 PPCPs were detected with the contents ranged from 0.058 to 0.127 μg/kg.The method is simple,solvent-saving,sensitive,accurate and stable.It is suitable for the simultaneous determination of PPCPs in sediment.