Simultaneous determination of 15 personal care products in human urine samples by using solid-phase exaction ultra-performance liquid chromatography tandem mass spectrometry
Simultaneous determination of 15 personal care products in human urine samples by using solid-phase exaction ultra-performance liquid chromatography tandem mass spectrometry
A method for simultaneous determination of 15 personal care products in human urine by solid-phase exaction ultra-performance liquid chromatography tandem mass spectrometry(SPE-UPLC-MS/MS)was established.The conditions for concentration of personal care products were optimized by investigating the extraction column,wash condition and elution condition.A volumne of 1mL urine was digested overnight by β-glucuronidase.The digested urine was loaded to Waters HLB(3cc/60 mg)solid phase extraction column.The sample was then washed by 1 mL of 25％(V/W)acetonitrile solution and eluted by 1.0 mL methanol twice.The elution solvent was blown to near dryness by nitrogen,and redissolved with 20％(V/W)acetonitrile solution with a final volumne of 1 mL.The purified sample was subjected to UPLC-MS/MS for analysis.Waters Acquity BEH C18 column(100 mm × 2.1 mm,1.7 μ m)was used for separation.The internal standard was used for quantification.The linear correlation coefficients of the 15 analytes were greater than 0.995,the limits of determination and the limits of quantification were within 0.005-0.24 ng·mL-1 and 0.017-0.8 ng·mL-1,respectively.The recoveries of the spiked samples were 80.0％-121％.The inter-day and intra-day relative standard deviations(RSDs)were 1.3％-7.7％and 3.7％-14％respectively.This method was applied to 95 urine samples collected from volunteers.The results revealed that methyl paraben(MeP),ethyl paraben(EtP),triclosan(TCS),and Triclocarban(TCC)had the highest detection rates(96％,56％,100％,and 100％,respectively).The mean detection concentrations were 4.11,0.69,0.52,5.12 and 1.95 ng·mL-1,respectively.The result was consistent with the reported literatures.The method established in this article has been verified by inter-laboratory and actual sample testing,and it is accurate,reliable,stable,easy to operate,and easy to promote in different laboratories.
关键词
个人护理品/固相萃取/超高效液相色谱-串联质谱/尿
Key words
personal care products/solid-phase extraction/ultra performance liquid chromatography-tandem mass spectrometry/urine
维普
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