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Journal of chromatography. B, Analytical technologies in the biomedical and life sciences v.1072, 2018년, pp.315 - 319   SCI SCIE
본 등재정보는 저널의 등재정보를 참고하여 보여주는 베타서비스로 정확한 논문의 등재여부는 등재기관에 확인하시기 바랍니다.

Quantification of glycocholic acid in human serum by stable isotope dilution ultra performance liquid chromatography electrospray ionization tandem mass spectrometry

Guo, Cheng (Cancer Institute (Key Laboratory of Cancer Prevention and Intervention, China National Ministry of Education), The Second Affiliated Hospital, Zhejiang University School of Medicine, Hangzhou, Zhejiang 310009, China ) ; Xie, Cong (Cancer Institute (Key Laboratory of Cancer Prevention and Intervention, China National Ministry of Education), The Second Affiliated Hospital, Zhejiang University School of Medicine, Hangzhou, Zhejiang 310009, China ) ; Ding, Peili (Cancer Institute (Key Laboratory of Cancer Prevention and Intervention, China National Ministry of Education), The Second Affiliated Hospital, Zhejiang University School of Medicine, Hangzhou, Zhejiang 310009, China ) ; Qin, Guangming (Department of Laboratory, The Second Affiliated Hospital, Zhejiang University School of Medicine, Hangzhou, Zhejiang 310009, China ) ; Mo, Weimin (College of Chemical Engineering, Zhejiang University of Technology, Hangzhou, Zhejiang 310014, China ) ; Cao, Xiaoji (College of Chemical Engineering, Zhejiang University of Technology, Hangzhou, Zhejiang 310014, China ) ; Zheng, Shu (Cancer ) ;
  • 초록  

    Abstract A rapid, accurate and sensitive stable isotope dilution ultra performance liquidchromatography electrospray ionization tandem mass spectrometry (ID-UPLC-ESI–MS/MS) method for the determination of glycocholic acid (GCA) in human serum was developed and validated. Serum samples were spiked with D 5 -glycocholic acid and then pretreated with protein precipitation. The analysis was performed on a Waters BEH C18 column (100 mm×2.1mm, 1.7μm), followed by ESI–MS/MS detection in negative ion mode under multiple reaction monitoring mode. The calibration curves covered a concentration range from 0.2 to 400ng/mL. The limit of detection and limit of quantification was 0.01ng/mL and 0.05ng/mL, respectively. The method showed satisfactory precision on intra-day (2.3–6.1%) and inter-day (2.4–4.6%) analyses and achieved good recovery at three spiked levels (103.7–114.3%). Moreover, this established method was successfully applied for quantification of GCA in serum samples from healthy volunteers, patients with hepatocellular carcinoma (HCC) and patients with other cancers. We demonstrated that the level of GCA in patients with HCC was significantly higher not only than that in healthy controls, but also than that in patients with other cancer, whereas no significant difference of GCA level was observed between healthy control group and other cancers group. Highlights A stable isotope dilution UPLC-ESI–MS/MS method for the detection of glycocholic acid was developed. The method was successfully applied to quantify glycocholic acid in human serum. 32 healthy volunteers, 10 patients with hepatocellular carcinoma and 14 patients with other cancers were recruited. Levels of glycocholic acid in patients with hepatocellular carcinoma were significantly increased.


  • 주제어

    ID-UPLC-ESI–MS/MS .   Glycocholic acid .   Serum .   Hepatocellular carcinoma .   Biomarker.  

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