• The performance of the method

– Limit of detection and quantification

– Sensitivity
– Specificity
– Recovery rate of the spiked standard
• Availability of instruments and reagents
• Cost and speed
• Compliance to government regulation (official
methods)
Official methods are rigorously tested and standardized.

AOAC International
– wide variety of foods, cosmetics etc.

American Association of Cereal Chemists (AACC)
– methods for cereal foods

American Oil Chemists' Society (AOCS)
– methods for oilseeds & high fat foods

International Union of Pure and Applied Chemists
(IUPAC)
– general food methods, non food

Cited by U.S. Code of Federal Regulation


Has rigorous validation procedure

Single-lab validation

Multiple-lab validation

Approval for First Action

Approval for Final Action

 Let’s revisit the Analytical Process
Food
Sampling Instrumentation Processing
Sample Interpretation
Pretreatment
Extraction
Separation
Clean up
Concentration
Derivatization

We cannot examine all of the products we are
interested in examining


Sampling is needed to take a portion of the entire
sample (population) for analysis


Analysis of the sample should provide an unbiased
estimation the population


May be the greatest source of error in your assay!
• Sample - Portion that represents the whole
• Population – Total quantity from which sample is obtained
• Sampling unit – units of counting for sample collection,
e.g. cans, boxes etc.
• Sample size – Number of sampling units in a sample
• Random sample - Just what it sounds like
• Lot – collection of units of the same size, type, style,
conditions, by same container code or same day
• Purpose – On-line processing control, quality
assessment of raw material, or nutrient analysis of end
products for labeling…
• Type and nature of food –
homogeneous/heterogeneous; milk, cereal, meat,
fruits…
• Nature of test – severity of risk associated with testing
results, cost, destructive/non-destructive …
FDA vs. USDA sampling procedures for nutrition labeling (Ch. 3)

FDA: (21 CRF § 101.9) “The sample for nutrient analysis

shall consist of a composite of 12 subsamples (consumer
units), taken 1 from each of 12 different randomly chosen
shipping cases, to be representative of a lot.”

USDA/FSIS: (9 CRF § 317.309) “The sample for nutrient

analysis shall consist of a composite of a minimum of 6
consumer units, each from a production lot.” “the units
may be individually analyzed and the results of the
analyses averaged, or the units would be composited and
the composite analyzed.”
Attribute sampling
• Sampling to measure absence or presence (+ or -) of a attribute
– Binomial distribution (ie. coin tossing), to make predictions
about the whole lot
– Example: Presence of C. Botulinum

Variable sampling
•Sampling to measure numerical values that change continuously
– Analytical data have normal distribution
–Example: Nutrient content requested by Nutrition labeling
• Single Sample Plan
– Acceptance based on one sample set
• Double Sample Plan
– One set, with the option of a second
• Multiple Sample Plan
– Must develop an acceptance chart
– Can be very costly
– You may NEVER reach a decision
7
6
5 Reject
4
REJECT
3
2
Keep Trying ACCEPT

1
0
Accept
-1
0 10 20 30 40
Non-Probability Sampling – non-random sampling
• Judgment (because I want this one)
• Convenience (because it’s easy)
• Restricted (because this is the only one I can get)
• Quota
Probability Sampling – random sampling
• Simple random
• Systematic
• Stratified
• Cluster
• Composite
• Each sampling unit in a population has the
equal chance to be sampled

• You have to know the number of units in your

population to give the equal chance

• Computer generated random number can be

used
 (Congressmen-election approach)

• Total population is divided into several regions or

strata
• Strata should be chosen to minimize variance within
strata and maximize variance between strata
• Can ensure a particular strata within a population
are adequately sampled and represented
• The sample size is usually proportional to the relative
size of the strata
(Congressmen-election approach)

Population 400

Regional population and

number of random samples
A 200 20
B 100 10
C 50 5
D 50 5
 (Congressmen vs. Senate)

Step 1: Divide population into regions or sub-groups

No difference

Step 2: Stratified, randomly select sample from each sub-groups

Quota, non-random sampling is made in sub-groups.
Personal judgment may be used for sampling
 (cluster then random selection)

Population 400, 50 cluster, 8 units per cluster

Systematic sampling
– Every nth after the first random sample
– Continuing sampling on a production line

Composite sampling
– Randomly select samples and combine them
–Example: FDA, USDA/FSIS procedure for nutrition labeling
 50 lbs
25 lbs

Laboratory 12.5 lbs

Sample
5g
• Particle size reduction
– Blending, chopping, mixing, pureeing etc.

• Packaging, freezing, heating, preservatives

• Prevent critical changes to sample

– Moisture loss, oxidation, enzyme action, MO growth
Will continue on Chapter 5

20