Quality Assurance Flashcards

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1
Q

What are different internal standards that can be used? (3)

A
  1. Same substance, but mass-labeled (or somehow different)
  2. Different substance (chemically similar)
  3. Same substance (spiking)
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2
Q

standard solutions have a known ____ and ____.

A

purity; concentration

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3
Q

What is a stock standard?

A

standard of HIGH CONCENTRATION, long storage life

- used to prepare working standards

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4
Q

A calibration curve is ____ _____ while spiking is ____ _____.

A

external calibration; internal calibration

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5
Q

When would a standard be determined to be expired?

A

The measurements of that standard differ from a newer standard by more than 10% (SANCO)

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6
Q

The storage condition of standards will affect:

A

stability/shelf life

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7
Q

True/False: stock standards are used for spiking, calibration, and comparison with samples during analysis

A

False; stock standards used to prepare working standards for that purpose

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8
Q

the linear relationship established by running standards should be:

A

a non-weighted regression curve (all points carry equal weight, do not force through intercept, etc)

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9
Q

What is the blank used for, in preparing an external calibration curve?

A

Subtract signal of blank from signal for each calibration point (correction)

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10
Q

How should the spacing and range of the standards be done, according to IUPAC?

A

spacing: depends on precision level required; should be evenly spaced
range: should be 0 to 150% of expected test result

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11
Q

How should calibration samples be run?

A

Random order

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12
Q

According to IUPAC, what is the minimum number of standards needed for a calibration curve?

A

5 (excluding 0)

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13
Q

What are residuals an indicator of?

A

Whether the calibration curve is acceptable

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14
Q

The residuals should be in what sort of distribution? What if this is not the case?

A

Randomly distributed around zero (regression curve of residuals is straight line y=0)
if TREND exists: problem with method, need to reexamine

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15
Q

List the steps of preparing an external calibration curve

A
  1. Prepare blank + standard samples (need triplicates)
  2. run in random order
  3. Calculate mean and SD for each point, correct using blank
  4. Graph and establish regression curve of best fit
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16
Q

What are residuals?

A

Difference between MEASURED value and CALCULATED value (using calibration curve)

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17
Q

What is the “linear range” of a signal on a calibration curve?

A

the concentration range at which SIGNAL INTENSITY is directly proportional to concentration (linear relationship)

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18
Q

(the blank signal + 3SD)/slope is the:

A

LOD

19
Q

What is IDL? What is MDL?

A

IDL: instrument detection limit
MDL: Method detection limit

20
Q

True/False: A good instrument should have a high LOD

A

False: a higher LOD means that it cannot detect lower concentrations confidently

21
Q

Differentiate IDL and MDL:

A

IDL: instrument limit, expressed as amount injected in machine for analysis; instrument blanks are run (only through machine)
MDL: for entire procedure, expressed as concentration in food matrix intially; procedural blanks are run (taken through all steps of procedure)

22
Q

What is LOQ? Define it.

A

limit of quantification
smallest level that can be quantified with acceptable precision/accuracy

10SD from concentration in procedural blank

23
Q

What is LOD? Define it.

what is the criteria?

A

Limit of Detection
smallest level that produces a SIGNIFICANTLY DIFFERENT signal from the background noise/blank
(can be distinguished/detected)

3SD from response obtained on blanks

24
Q

If the result is below the LOD, what do you do?

A

report as below LOD

25
Q

Procedural blanks are also known as:

A

matrix blanks

26
Q

Why might calibration curves prepared using standard samples be inaccurate for comparison with a food sample?

A

Matrix effect; calibration curve does not correspond to signal obtained from food sample

27
Q

Spiking is known as the:

A

standard addition method

28
Q

What do you report if the result is above LOD but below LOQ?

A

signal is sufficient to indicate presence (detectable), but not enough to be quantified.
Report as BELOW LOQ

29
Q

Can a result be above the LOQ but not the LOD?

A

No. LOD < LOQ

30
Q

How can the matrix affect the analysis results?

A

Increase or decrease signal, give higher or lower concentrations than actual amounts

31
Q

You can only report the level of the analyte if the result was above both the ____ and the ____.

A

LOD, LOQ

32
Q

The spiking solution added should be: (2)

A
  • small amount (assume volume stays constant)

- highly concentrated (so can add small amount)

33
Q

What is the standard addition method?

A

Add KNOWN AMOUNTS of standard solution (same as analyte) to sample -> measure response before/after each addition (x, x+1, x+2, x+3…) -> establish curve, determine original amount (x)

Or, can separate sample into many SUBSAMPLES, add increasing amounts to each

34
Q

What is the internal standard method?

A

Adding fixed amount of ANOTHER CHEMICAL to sample

35
Q

The ____ is the same over a range of concentrations, which is used in internal standard calculations.

A

RF (response factor)

36
Q

The substance added in the internal standard method should: (2)

A

have similar chemical properties

Not interfere with analyte analysis

37
Q

The internal standard method aims to deal with: (3)

A

Matrix effect
Injection variability
Analyte loss

38
Q

What is used as an IS in ICP-MS?

A

rare elements (Yttrium, Rhodium, Indium, Scandium)

39
Q

What could we use as an IS in GC-MS or LC-MS?

A

Mass labelled surrogate

40
Q

what is the response factor?

A

ratio of (signal A/IS) / (concentration A/IS)

41
Q

“Trueness” is also known as ____. How do you assess it? (4)

A

Recovery

  1. Comparison of results with known standard (certified ref material)
  2. Compare results with those from a method that works, has little error
  3. compare with results from interlaboratory tests
  4. spiking samples (based on blanks or positive blanks)
42
Q

Where can you source certified materials in Canada? In the US?

A

Canada: NRC Certified Reference Materials
US: NIST

43
Q

What is mass labelling?

A

Using a modified version of the compound, with C13 or deuterium instead of normal C or H (molecule will have different molecular mass, so can be differentiated from original)