Analysis and testing Flashcards
What is analytical method transfer? How do you transfer assay of a tablet?
Analytical Method transfer from India to UK
Discussed ICH Q 14
Where would you find guidance on how to validate chromatographic testing methods (HPLC)
Can you describe the parameters that would be validated for an HPLC method? and what stats tool you’d use?
Accuracy
Linearity
Precision
Specificity
Range
Robustness
Limit of Detection
Limit of Quantitation
Solution stability
You are working as a QP at a site and have been asked to support your QC team in carrying out method transfer of a HPLC method. How would you go about this?
comparative testing
Any other types of method transfer other than comparative testing?
Stability assay is OOS (one in spec one slightly out of spec); batches on the market; what do you do? Oncology drug everything else is in spec.
; discussion around recall types
MHRA OOS guidance - tell me the process
dissolution failure
You are moving testing from a site in India to UK – how would you do this?
After completion of method transfer there is an OOS on the first batch tested in UK lab but Indian lab is showing passing result – what do you do?
Give examples of what you would look at in Phase 1a/b?
Turns out it’s a true OOS – can you release the batch?
That batch was scrapped and we released another batch, 3 months later there is an OOT for an impurity – what are your thoughts?
Describe the recall procedure .
You have a stability batch and there was an oos at 18 months for Tablet, shelf life was 24 months. Cancer drug.
Why will you not reject this batch when I said I will not, then justify – cancer drug
A routine stability batch OOT for assay at 18 months for another product, which drilled more detailed about the concern with MDI.
What confidence interval, its calculation and why do you keep 95% confidence interval?
How would you set up a stability programme for a tablet product?
Where would you find guidance bracketing and matrixing ? Can you please explain what do they mean?
You receive a call on Friday evening from QC informing about OOT for tablet assay testing at 9 months. Shelf life is 36months. What are your concerns?
You have now been told that batch will fail at 12 months. What do you do?
Which type of stats would you use to estimate shelf life?
I drew a graph to explain this and the assessor was happy.
Are you allowed to perform extrapolation?
How would you perform a method transfer of Assay method to another lab? What stats would you use?
What are the difference between biological and chemical tests methods?
Please explain what ELISA is?
What statistical methods would you use for chemical and biological analysis with examples?
HPLC for unknown impurity at 0.1%, OOS at 18 months stability, what do you do? Shelf life is 24 months
How will you calculate potency in a cell based product, how will you go about to test robustness in ELSIA method and what stats will you use in the case you want to test the following:
*Different temperatures
*Different incubation times
*Different dyes
Difference between biological and chemical methods
a beta blocker product stability batch fail at 18M:
*What is the OOS/OOT procedure?
Explain HPLC analysis and instrumentation?
What is regression analysis
tell us Packaging line IPC checks
Tell us Recall procedure
and Types of recall?
Your lab informs you of a related substance peak at 12M on a stability trial that is unexpected. What are you going to do?
Where is the guidance for OOS investigations? How would you conduct one?
OOT at 6 months for impurity for Solid Oral Dose
Phase 1a/1b investigation – asked for specifics of what would be required
Phase 2 – no issues at DP manufacturing site
API site had reworked the batch
What documentation would you expect for rework?
What is the difference between reprocessing and rework?
Considerations for market action
You receive a call from your QC lab you have an OOS and an OOT for a low assay result on a dry powder inhaler product it’s for a 12 month stability time point - what do you do?
a. Further information on questioning – 2 sets of assay results one OOT and one OOS, but mean within specification and the mean is what has been registered
b. Discussed other time points, all ok
c. Discussed other tests – expelled dose was also low 73% - medical have advised no lack of efficacy would be noted
d. No increase in complaints from PV
e. Asked about market – informed that all batch is used within 3-4 months of being certified and placed on market
f. Went through oos/t investigation
g. Phase 2 found out that maintenance on the sealing jaws of the dpi tablet sealing during batch - wasn’t sealing correctly
h. Temperature was high
i. Some unsealed / some too high temp exposure
j. Went into recall for any remaining stock on the market
You receive a call that a tablet on stability has failed dissolution stage 1
a. Went through OOS/T – were interested in phase 2 investigation
b. Went through investigation and potential probable root causes
c. Stopped me at API as had another scenario later on this
.
What is analytical method transfer?
How do you transfer assay of a tablet?
Explain T test in detail
