Application of PULCON to purity assay of Acetaminophen

  • Summary


There are various methods of qNMR analysis which are internal standard method and external standard method. An Internal standard method is carried out qNMR using analytical sample that contains reference material. In the case of external standard method, solution of reference material is prepared and NMR measurement is conducted analyte and reference standard sample Individually.

What is PULCON?

PULCON is one of the external standard methods. It stands
for Pulse length based concentration determination.
PULCON is a quantification that is performed to compare
NMR spectrum between analyte and reference material

A signal intensity has a correlation between obtained NMR
spectrum based on equation 1. To consider factors such as
pulse width , measurement temperature and receiver gain,
calibration of measurement and calculation are carried out.


Confirmation of linearity

To prepare for a variety concentration of NMR sample s that
are BTMSB-d4 of DMSO-d6 solution , the correlation between
measurement values and preparation values are confirmed.

Measurement condition
Sample concentration:0.06mM , 0.25mM , 0.99mM , 3.96mM

The measurement values correspond to prepared values , these
results have a response of linearity.

*It is mentioned PULCON has much more bias factors that
affect results such as instrument or sample tube than internal
standard method.

Application to purity assay of Acetaminophen

STEP1:Sample Preparation

Solution of analyte:Acetaminophen in DMSO-d6 was
prepared in JEOL lab.

Solution of reference material
:15mM Benzoic acid in DMSO-d6 was purchased from CIL
(Product number :DLM-7061C)
※This reference solution is suitable for external standard ethod
ecause it has a certification of mol concentration with SI traceability.

STEP2:NMR measurement


Data processing and reduction on Delta NMR software


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