Monday, August 22, 2011

tM for hilic column

UN-retained compounds pass through tubes and and column t0 (units of time), the volumn of system plus the void volumn column,
The ICP-MS used V(tube and connector) = 0.05 mL small.
For example to determine the tM, using ICP-MS, the column is Zic-Hilic, the hydrophobic compound containing Platin is analyzed.
Inorganic platin is mixed with Sodium diethyldithiocarbamate trihydrate (DDTC)
  • (C2H5)2NCSSNa · 3H2O
  • Molecular Weight: 225.31


in buffer pH = 9.
the proportion: 100ppb/1000ppb
the reaction occurred around 30min
inject the mix to ICP-MS, change Zic-hiclic column, pc-hilic column
- used sulfur containing compounds which is not retained by zic-hilic column to determine the tM value
for example:

2-Methylbenzenethiol: Due to the small electronegativity difference between sulfur and hydrogen, an S-H bond is practically nonpolar covalent.  Therefore, the S-H bond in the thiols have a lower dipole moment as compared to the alcohol's O-H bond.  Thiols show little association by hydrogen bonding, with both water molecules and among themselves.  Hence, they have lower boiling points and are less soluble in water and other polar solvents than alcohols of similar molecular weight.  Thiols are as soluble and have similar boiling points to isomeric sulfides.

Methyl phenyl sulfide

  • Synonym: Methyl phenyl sulfide, Thioanisole
    • Linear Formula: C6H5SCH3
    • Molecular Weight: 124.20
    • CAS Number: 100-68-5
      the purchased tioanisol 25mM = 3000ppm

      Mixture of 10ppm cisplatin and C6H5SCH3 is analyzed to determine the tM.
      Change the instrument set up to detect SO+ isotop
      Reaction cell B, 
      using Standard mode, turn to DCR mode.
      to give a good signal from S the concentration of tioanisol should be 300 ppb or 600 ppb
      1. column ZIC-HILIC
      2. Change the column: N-C-C-C-PO4-
      HPLC prepacked column HPLC from GENETEC  and http://www.mn-net.com/
      the same eluent:  2.5% 1-propanol in 5 mM ammonium acetate.
      3. Using column PC-HILIC (4.6 mm i.d, x100mm, 5um)from http://www.shiseido.co.jp/
      back pressure 6,

      Phosphorylcholine (PC) is a partial structure of phosphatidylcholine (lecitin), one of the phospholipids forming cell membranes. PC has a betaine structure and shows high hydrophilicity, biocompatibility, and inhibitory effect of protein adhesion. Its superhydrophilic character is suitable to the application as a HILIC phase.
       



      Chemical structure of PC

 






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