PMID- 31875826
OWN - NLM
STAT- MEDLINE
DCOM- 20200114
LR  - 20200114
IS  - 1000-8020 (Print)
IS  - 1000-8020 (Linking)
VI  - 48
IP  - 6
DP  - 2019 Nov
TI  - [Determination of 25-hydroxyl vitamin D in serum by isotope dilution ultra-fast 
      liquid chromatography-tandem mass spectrometry].
PG  - 981-987
AB  - OBJECTIVE: To establish a rapid and accurate method for determination of 
      25-hydroxyl vitamin D2, 25-hydroxyl vitamin D3 and 3-epi-25-hydroxyl vitamin D3 
      in serum by isotope dilution ultra-fast liquid chromatography-tandem mass 
      spectrometry(UFLC-MS/MS). METHODS: The serum sample was extracted by nhexane 
      after methanol/acetonitrile precipitation protein, and then the extract was 
      concentrated by nitrogen and volumed with the primary mobile phase. The 
      chromatographic separation was carried out on a Phenomenex Kinetex F5 column(2. 1 
      mm x 150 mm, 1. 7 mum) by using 0. 1%(V/V) formic acid and 0. 1%(V/V) formic 
      acid/methanol solution as the mobile phase with the gradient elution. Detection 
      was performed in positive multi-reaction monitoring(MRM) mode with the isotope 
      internal labeling method for quantification. RESULTS: The baseline separation was 
      obtained within 6 min for the epimer 25-hydroxyl vitamin D3 and 3-epi-25-hydroxyl 
      vitamin D3, and the accurate qualification was obtained for the simultaneous 
      determination of 25-hydroxyl vitamin D2, 25-hydroxyl vitamin D3 and 
      3-epi-25-hydroxyl vitamin D3. The three analytes showed good linear relationship 
      within the range of 0. 5-50. 0 mug/L with a correlation coefficient r >0. 9995. 
      The limits of detection(LODs) and the limits of quantitation(LOQs) of the method 
      were 0. 15 mug/L and 0. 5 mug/L, respectively. The recoveries of the method were84. 
      3%-109. 0%(n = 11) at the three spiked levels of 1. 0, 10. 0 and 30. 0 mug/L, and 
      the relative standard deviations(RSDs) were between 0. 8%-6. 8%. At the same 
      time, the certified standard reference materials(SRM) of the America National 
      Institute of Standards and Technology(NIST) Level 1, Level 2, Level 3 and Level 
      4(SRM 972 a)were used as the quality control samples for verification, the 
      relative deviations of the measurement result were less than 5% compared with the 
      reference values. CONCLUSION: The developed method has the characteristics of 
      simplicity, rapidity, sensitivity and accuracy, and is suitable for the 
      simultaneous rapid determination of 25-hydroxyl vitamin D2, 25-hydroxyl vitamin 
      D3 and 3-epi-25-hydroxyl vitamin D3 in serum.
FAU - Chen, Xiaohong
AU  - Chen X
AD  - Key Laboratory of Health Risk Appraisal for Trace Toxic Chemicals of Zhejiang 
      Province, Ningbo Municipal Center for Disease Control and Prevention, Ningbo 
      315010, China.
FAU - Zhou, Jian
AU  - Zhou J
AD  - Key Laboratory of Health Risk Appraisal for Trace Toxic Chemicals of Zhejiang 
      Province, Ningbo Municipal Center for Disease Control and Prevention, Ningbo 
      315010, China.
FAU - Jin, Micong
AU  - Jin M
AD  - Key Laboratory of Health Risk Appraisal for Trace Toxic Chemicals of Zhejiang 
      Province, Ningbo Municipal Center for Disease Control and Prevention, Ningbo 
      315010, China.
LA  - chi
PT  - Journal Article
PL  - China
TA  - Wei Sheng Yan Jiu
JT  - Wei sheng yan jiu = Journal of hygiene research
JID - 9426367
RN  - 0 (Isotopes)
RN  - 1406-16-2 (Vitamin D)
SB  - IM
MH  - Chromatography, High Pressure Liquid
MH  - Chromatography, Liquid
MH  - Isotopes
MH  - *Tandem Mass Spectrometry
MH  - Vitamin D
OTO - NOTNLM
OT  - 25-hydroxyl vitamin D_2
OT  - 25-hydroxyl vitamin D_3
OT  - 3-epi-25-hydroxyl vitamin D_3
OT  - UFLC-MS/MS
OT  - epimer
OT  - isotopic internal standard method
OT  - serum
EDAT- 2019/12/27 06:00
MHDA- 2020/01/15 06:00
CRDT- 2019/12/27 06:00
PHST- 2019/12/27 06:00 [entrez]
PHST- 2019/12/27 06:00 [pubmed]
PHST- 2020/01/15 06:00 [medline]
PST - ppublish
SO  - Wei Sheng Yan Jiu. 2019 Nov;48(6):981-987.