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  1. #1

    Default recovery in method validation

    IN assay by HPLC method validation,recovery(accuracy) parameter required or not?

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  3. #2

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    Quote Originally Posted by srinivas2202 View Post
    IN assay by HPLC method validation,recovery(accuracy) parameter required or not?
    Yes it is required!!!! Please check ICH Q2R1.
    Dr. Shahid A Syed
    QA/Validation Specialist
    Penn Pharmaceutical
    www.pennpharm.com

  4. #3

    Default

    Quote Originally Posted by srinivas2202 View Post
    IN assay by HPLC method validation,recovery(accuracy) parameter required or not?
    Yes it is required!!!! Please check ICH Q2R1. I want to give one input here, if you are dealing with family validation (Method validation for 2 or three strengths) and if there is no major difference in fromulation except some variation in excepients quantities then you can perform full validation parameter for one strength and for the other strength you can go with limited parameters like Specificity and precision repeatability, but a comprehensive report of full validation should be attached with the report of other strengths as a ready reference.
    Dr. Shahid A Syed
    QA/Validation Specialist
    Penn Pharmaceutical
    www.pennpharm.com

  5. #4

    Default

    Quote Originally Posted by srinivas2202 View Post
    IN assay by HPLC method validation,recovery(accuracy) parameter required or not?
    Dear Srinivas,

    Assay
    Drug Substance
    Several methods of determining accuracy are available:
    a) application of an analytical procedure to an analyte of known purity (e.g. reference material);
    b) comparison of the results of the proposed analytical procedure with those of a second well-characterized procedure, the accuracy of which is stated and/or defined.
    c) accuracy may be inferred once precision, linearity and specificity have been established.
    Drug Product
    Several methods for determining accuracy are available:
    a) application of the analytical procedure to synthetic mixtures of the drug product components to which known quantities of the drug substance to be analysed have been added.
    b) in cases where it is impossible to obtain samples of all drug product components , it may be acceptable either to add known quantities of the analyte to the drug product or to compare the results obtained from a second, well characterized procedure, the accuracy of which is stated and/or defined (independent procedure,accuracy may be inferred once precision, linearity and specificity have been established.(Ref ICH Q2R1)
    Shahnawaz Sajid (Ph.D)

  6. #5

    Default recovery in method validation

    Dear sir,

    Actually we are validating the api producut.please avise me how i can perform the recovery in assay validation with any example.

    Rgds
    Vasu

  7. #6

    Default

    Quote Originally Posted by srinivas2202 View Post
    Dear sir,

    Actually we are validating the api producut.please avise me how i can perform the recovery in assay validation with any example.

    Rgds
    Vasu
    Dear Srivas,
    Analytical methods for API should be validated unless the method employed is included in the relevant pharmacopoeia or other recognised standard reference. Methods should be validated to include consideration of characteristics included within the any recognized guidelines on validation of analytical methods. The degree of analytical validation performed should reflect the purpose of the analysis and the stage of the API production process.

    Thanks
    Shahnawaz Sajid (Ph.D)

  8. #7
    prabhakar
    Guest

    Default

    Actually we are performing Accuracy like this for API Assay validation

    From linearity exercise you can calculate C i.e y-intercept

    Y=mX+C

    where m= slope
    C- Y intercept
    Y-Response
    X-Concentration

    Therefore

    X=(Y/m)-C

    You know X (theoritical ) value from the theoritical dilution or from the weight taken and you can calculate the X (Experimental) value from the above formula from the graph.

    Accuracy = X(Experimental)/X(theoritical) X 100

    As an additional acceptance criteria You can add Residual sum squares also .

  9. #8

    Default recovery in method validation

    ThanQ sir.

    actually i asked not about calculation part.which compound is spiking with standard solution when standard and sample as same concentration.(i mean impurity or sample)


    Rgds
    vasu

  10. #9

    Default

    HI,

    Yes its really need to the validation its very important to the recovery process the accuracy level is increased that should be the increase the recovering of the addictors level.

    Thank you...

  11. #10

    Default prepration of accuracy solution for impurity validation in API

    if known imp limit is NMT0.1% and total rs is nmt 0.5% and sample conc.is 1mg/ml.then how i will prepare 80%,100%,120% recovery solution by spiking the imp.is there any criteria for that.

  12. #11
    Validation Analyst
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    Default recovery

    It is the riboflavin test requered to demonstrate recovery of the sprayballs??

  13. #12
    Validation Analyst
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    Unhappy coverage

    there is a regulation to explain how to do that?:

  14. #13

    Default

    suppose i am doing validation for api, no impurity is using in the analysis. Then how we perform recovery

  15. #14

    Default API accuracy in validation by linearity plot

    Quote Originally Posted by prabhakar View Post
    Actually we are performing Accuracy like this for API Assay validation

    From linearity exercise you can calculate C i.e y-intercept

    Y=mX+C

    where m= slope
    C- Y intercept
    Y-Response
    X-Concentration

    Therefore

    X=(Y/m)-C

    You know X (theoritical ) value from the theoritical dilution or from the weight taken and you can calculate the X (Experimental) value from the above formula from the graph.

    Accuracy = X(Experimental)/X(theoritical) X 100

    As an additional acceptance criteria You can add Residual sum squares also .
    When you do this,
    1. would you do linearity and accuracy test on the same run, can you do it on separate runs as well?
    2. if the same run, would you use accuracy samples in generating linearity plot?
    3. if the linearity pass (eg. r>0.999), is there any possibility accuracy can fail (provided, samples and testing have no errors)?
    thanks,
    ranjith

  16. #15
    Validation Guru
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    Default

    call me on 9676749937.
    Bujji Reddy Kanchi.

  17. #16
    Validation Guru
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    Default

    1.why to to seperately. both linearity and accuracy in single sample set.

    consider linearity solutions are standards for accuracy samples for the recovery calculation.
    2.No need to establish linearity(correlation coefficient) for accuracy study.
    3.Once linearity passess. accuracy will definitely pass.

  18. #17
    Validation Guru
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    Default

    Its better not to conduct for Validation for Related substances test. If no impurities is available.

    Forced degradation study is enough for that method.

  19. #18
    Validation Guru
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    Default

    Always spike the impurity stock solutions rather than impurity standard solutions.

    Usually There is no possibility of having standard and Test sample having same concentrations.

  20. #19
    Validation Guru
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    Default

    Quote Originally Posted by suneel.dutt View Post
    if known imp limit is NMT0.1% and total rs is nmt 0.5% and sample conc.is 1mg/ml.then how i will prepare 80%,100%,120% recovery solution by spiking the imp.is there any criteria for that.
    Good Question

    For eg:
    Test preparaton(1mg/ml)= 100mg /100 ml (which gives 1mg/ml concentration)
    Impurity Standard(0.001mg/ml) = 1 mg /100 ml (this is stock solution)
    Dilute 10 ml of stock to 100ml with diluent.

    Preparation of 80% Recovery solution =
    weigh 100 mg of test sample into a 100mL volumetric flask. add 8 ml of stock solution then make up to 100ml with diluent.


    Preparation of 100% Recovery solution =
    weigh 100 mg of test sample into a 100mL volumetric flask. add 10 ml of stock solution then make up to 100ml with diluent


    Preparation of 150% Recovery solution =
    weigh 100 mg of test sample into a 100mL volumetric flask. add 15 ml of stock solution then make up to 100ml with diluent.


    Acceptance Criteria :85% to 115% to the theoretical amount added

  21. #20

    Default

    Quote Originally Posted by bujjikanchi View Post
    Good Question

    For eg:
    Test preparaton(1mg/ml)= 100mg /100 ml (which gives 1mg/ml concentration)
    Impurity Standard(0.001mg/ml) = 1 mg /100 ml (this is stock solution)
    Dilute 10 ml of stock to 100ml with diluent.

    Preparation of 80% Recovery solution =
    weigh 100 mg of test sample into a 100mL volumetric flask. add 8 ml of stock solution then make up to 100ml with diluent.


    Preparation of 100% Recovery solution =
    weigh 100 mg of test sample into a 100mL volumetric flask. add 10 ml of stock solution then make up to 100ml with diluent


    Preparation of 150% Recovery solution =
    weigh 100 mg of test sample into a 100mL volumetric flask. add 15 ml of stock solution then make up to 100ml with diluent.


    Acceptance Criteria :85% to 115% to the theoretical amount added
    What will be the validation range? 80% to 150% of standard concentration level? Can you report if you found impurity at a level outside this? How about using lower level at LOQ rather than 80%. This can extend the validation range.

  22. #21
    Validation Guru
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    Default

    if no impurity is available. stop doing validation.

  23. #22

    Default Calculating Recovery using pre-existing amount

    I have a question regarding the calculation of recovery when there is a pre-existing amount of analyte in the sample. We have two schools of thought on how to calculate this....wondering what the general consensus is...

    1) %Recovery= ((Actual calculated amount in recovery sample)/(Amount Spiked into the recovery sample+ calculated theoretical pre-existing amount (determined from unspiked sample evaluation)) )x 100%

    2) %Recovery=((Actual calculated amount in recovery sample - Calculated theoretical pre-existing amount)/ (Amount Spiked into the recovery sample)) x 100%

    Thanks....

  24. #23
    Validation Guru
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    No,it is an example for understanding preparations only,

    for impurities the lower concentration must be from LOQ Level, but not 80%.

    the validation range in case of impurities should be LOQ Level to 150% of the specification.

    80 to 150% or 120% levels normally followed in assay of major analyte

  25. #24

    Default

    i'am waiting for the answer to this as well

  26. #25
    Validation Guru
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    Default

    correct method of calculation

    %Recovery=((Actual calculated amount in recovery sample - Calculated theoretical pre-existing amount)/ (Amount Spiked into the recovery sample)) x 100%


    Regards,
    Bujji reddy k

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