CCK Discussion Forum on Impurity Emergence: A Wake Up Call for Drug Safety & Quality - 13 Oct 2019 at ICCBS, University of Karachi. Session largely participated by qualified and experienced pharmaceutical professionals having diversified educational background and experience.

1. Analytical
Techniques & its
Reliability
CCK- Forum
Sunday, Oct 13th Karachi
Lecture
2

3. Analytical Techniques & its Reliability

4. Ultraviolet
Spectroscopy

5. Liquid
Chromatography

10. Mass
Spectroscopy

11. Mass Spectroscopy
Ionized atom or molecule
Molecular masses & charges
Separate & detect based on

12. Mass Spectroscopy
Vaporization
Ionization

13. Mass Spectroscopy
If it is
temperature
sensitive

14. Mass Spectroscopy
Direct infusion
If it is
temperature
sensitive

15. LC - MS
Reduce experimental error
Improves accuracy

16. LC - MS
Separate mixture in accordance
with their physical & chemical
properties
Detecting based on their mass
spectrum
Identifying the components within
each peak

18. Lets connect with Impurities
NDMA

19. What it is
? Yellow Odorless liquid
It was used to make rocket fuel
Unintentionally formed in air,
water, soil during various
manufacturing reactions
involving alkyl amines
Alkyl Amine
Widely distributed throughout
the environment

20. What it is
?
NDMA
Does not persist in the environment, break
down in sunlight in minutes

21. it enters in the human bodyHow
Breathe ContactEat Drink
Enters Blood & goes to many body organs in
minutes
Metabolize in Liver and leave the body within
24 hours through Lungs & Urine
?
?

22. NDMA crippled
Recall Thunders and Concerns

23. LC-MS - NDMA
LOD 0.3 ng/ml
Range 1 to 100 ng/ml
LOQ 1 ng/ml

24. Principle
Separated by Reverse Phase
Based on m/z value of protonated
impurity ion
Detected by Mass
Spectrophotometer
NDMA from
Ranitidine

25. Principle
Flow rate 0.5 ml/min
Column temperature 30℃
Column C18, 3 um (50x4.6 mm)
Injection volume 3 uL
Temperature 4 to 8℃
NDMA from
Ranitidine

26. Thank You