Food Sampling Technique

To control food quality and acceptance within satisfactory limits, it is important to monitor
the vital characteristics of raw materials, ingredients, and processed foods. This could be
done by evaluating all foods or ingredients from a particular lot, which is feasible if the
analytical technique is rapid and non-destructive. However, it is usually more practical to
select a portion of the total product volume and assume the quality of the selected portion
is typical of the whole lot. Obtaining a portion, or sample, that is representative of the
whole is referred to as sampling, and the total quantity from which a sample is obtained is
called the population.
Acceptance sampling is the plan to control the quality of the product after the production
is complete. The plan is based on a systematic plan that decides how to sample the finished
goods so as to maintain the quality at desired level. It is also used for incoming material or
parts and based on the acceptance sampling plan it is decided to accept or reject the whole
lot or batch of items, similarly for finished product.

Acceptance sampling is a statistical method that enables us to base the accept – reject
decision on the inspection of a sample of items from the lot.
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 Food Sampling Technique

Homogeneous and heterogeneous population

The ideal population would be uniform throughout and identical at all locations. Such a
population would be homogeneous. Sampling from such a population is simple, as a sample
can be taken from any location and the analytical data obtained will be representative of the
whole.
However, this occurs rarely, as even in an apparently uniform product, such as sugar syrup,
suspended particles and sediments in a few places may render the population heterogeneous.
In fact, most populations that are sampled are heterogeneous. In other words, it consists of
elements that are not of the same kind or nature

Therefore, the location within a population where a sample is taken will affect the subsequent
data obtained. However, sampling plans and sample preparation can make the sample
representative of the population or take heterogeneity into account in some other way.

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 Food Sampling Technique
Storage and Preservation of Samples

Prepared samples may undergo changes in composition through evaporation or absorption

of moisture or by the action of enzymes or microorganisms. The components that are
likely to change for e.g, ascorbic acid should be analyzed immediately after preparation in
fresh material. Products which are likely to undergo microbial spoilage may be preserved
by using preservatives or by freezing or by drying.  
1. Drying: Sample containing moisture can be dried as rapid and at as low a temperature
possible. Spreading the sample over a wide area can facilitate drying. Generally, drying at
60 º C under vacuum is recommended. If the sample contain no heat ‐ sensitive or volatile
compounds, heating for several minutes at 70 to 80 º C may be advisable. Such heating
also inactivates most enzymes. During drying, certain components are destroyed
(enzymes, vitamins), other are almost invariably modified (proteins and lipids) and some
flavour components are volatilized. If drying is not done carefully, ceramelization and
sugar inversion in acid foods are likely to occur.  

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 Food Sampling Technique
2. Freezing: Some plant materials can be stored at ‐20 to ‐30º C provided they can be
cooled to low temperature within 1 h. Freezing of samples in air and moisture proof
containers by rapid freezing and storage at less than ‐6.7º C prevents microbial activity but
not the enzyme activity which continues to occur at temperature down to ‐40º C, although it
a slower rate. Plant acid phosphatases function at ‐28º C in frozen state, so, issues or extracts
for studies of phosphate metabolism can be stored in the cold after drying. Most foods are
preserved best by freeze‐drying. Fresh foods, in which enzymes have not been inactivated
prior to freezing, are especially susceptible enzymatic attack during and after thawing.  
Polyunsaturated fatty acid are less damaged when stored in frozen (‐20ºC) intact tissues than
after they are extracted from the tissues. Storage of dried products at 0 to 10ºC minimizes
deterioration. To minimize oxidative changes, preservation at low temperatures under
nitrogen is recommended for most foods. Storage and hermetically closed containers reduce
compositional changes of relatively dry foods at about 40º C. While taking samples, stored
at low temperature for analysis either entire container should be warmed to room
temperature or a portion transferred quickly to a clean, dry stoppered container to avoid
change in moisture content. 4
Sample rich in lipids must be chilled rapidly prior to extraction or frozen quickly for storage.
 Food Sampling Technique

3. Chemical: Dry fat samples should be stored under nitrogen or dissolved in petroleum
ether. Storage in ethyl ether is undesirable because it tends to form oxidative peroxides.
Dilution with petroleum ether and flushing in a stream of pure nitrogen is a good practice
for temporary protection.
Addition of antioxidants (0.1‐ 0.05% of Propyl gallate or santoquin) is effective provided it
does not interfere with the analytical determinations.  To reduce or eliminate microbial
attack, preservatives such as sorbic acid, sodium benzoate, sodium salicylate, tyrosin,
formaldehyde, mercuric chloride, toluene, or thymol are used. Selection of preservatives,
however, will depend upon the nature of food, expected contamination, storage period and
analysis to be performed.   All prepared food samples should be rapidly transferred to dry
glass or plastic containers with well‐fitted lid, clearly labeled and stored at a suitable low
temperature.

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 Food Sampling Technique
Sampling Errors  
Sampling errors are caused by several factors. Lack of randomness in sample selection
may result from either instrumental limitations or deficiencies and from human bias.
Manual methods of sampling powdered or granular materials are subject to numerous
errors. Baker et al. (1967) studied the factors that bias sampling by triers. These factors
include:
 Particle shape‐round particles flow into the sampler compartments more readily than
angular particles of similar size;  
 Surface adhesiveness ‐ an uncoated hygroscopic material flows into the sampler
compartment more readily than non – hygroscopic materials of similar shape and of
either larger or smaller size; and  
 Differential downward movement of particles (on the basis of size) when disturbed
during sampling.  
Changes in composition may occur during or after sampling. Typical changes include
gain or loss of water, loss of volatiles, physical inclusion of gases, reaction with container
material or foreign matter in container, and damage to fruits or vegetables by mechanical
injury leading to enhanced enzymatic or chemical changes.  6
 Food Sampling Technique
The main problem arises, however, from the non – homogeneity of many foods. Both
macro – heterogeneity and micro – heterogeneity are common. The latter is especially
important in determinations of vitamins and other minor components. For example,
nicotinic acid and thiamine are concentrated in wheat kernel; epidermis cells of grapes
are rich in anthocyanin pigments; and essential oils in citrus fruits are mainly in cells of
the flavedo layer. But major components also are distributed unevenly. Proteins, lipids,
minerals, and crude fiber are higher in the outer layers than in the endosperm of cereal
grains; variations in water, sugars, and organic acids are found in various tissues of fruits
and vegetables; and the uneven distribution of fat in meat makes it imperative to express
some analytical values on a fat ‐ free basis.   Most of these difficulties are overcome by
fine grinding and mixing of large samples. In some instances, however, attempts to
homogenize a food sample are wrought with difficulties; in others, apparently
homogeneous preparations have a tendency to segregate or stratify. Failure to recognize
and appraise the variations in a sample may limit or even invalidate conclusions from
analytical data.   To summarize, the aim of sampling is to secure a portion of the material
that satisfactorily represents the whole. The more heterogeneous the material, the greater
the difficulties and required efforts to obtain a truly representative sample. 7
 Food Sampling Technique
Sampling Technique
There are several sampling methods/techniques in common use. These are probability
sampling, non-probability sampling, bulk sampling, and acceptance sampling. These are
described in brief below:
Probability sampling
Probability sampling is used when a representative sample is desired, and uses principles of
statistical sampling and probability i.e. elimination of human bias. It is a random selection
approach that tends to give each unit an equal chance of being selected.
Simple random sampling requires that the number of units in the population be known and
each unit is assigned a number. A specific quantity of random numbers between one and total
number of population units is selected. Units corresponding to the random numbers are then
analyzed as an estimate of the population.
Systematic sampling is used when a complete list of sample units is not available, but when
samples are distributed evenly over time or space, such as on a production line. The first
sample is selected at random and then every nth unit after that.
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 Food Sampling Technique

Stratified sampling involves dividing the population into overlapping subgroups so that
each subgroup is as homogenous as possible. Random samples are then taken from each
subgroup. The procedure provides a representative sample because no part of the population
is excluded.
Cluster sampling entails dividing the population into clusters or subgroups so that cluster’s
characteristics are as identical as possible, that is, the means are very similar to each other.
Any heterogeneity occurs within each cluster. The clusters are sampled randomly and may be
either totally inspected or subsampled for analysis.
Composite sampling is used to obtain samples from bagged products such as flour, seeds,
and larger items in bulk. Two or more samples are combined to obtain one sample for
analysis that reduces differences between samples. For example, FDA composite 12 and at
least six subsamples, respectively, for the sample to be analyzed for compliance with
nutrition labeling regulations.

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 Food Sampling Technique
Non-probability Sampling
Non-probability sampling is used when it is not possible to collect a representative sample, or
a representative sample is not desired. For example, in case of adulteration such as rodent
contamination, the objective of the sampling plan may be to highlight the adulteration rather
than collect a representative sample of the population.
Judgement sampling is solely at the discretion of the sampler and therefore is highly
dependent on the person taking the sample. This method is used when it is the only practical
way of obtaining the sample.
Convenience sampling is performed when ease of sampling is the key factor. The first pallet
in a lot or the sample that is most accessible is selected. This type of sampling will not be
representative of the population, and therefore is not recommended.
Restricted sampling may be unavoidable when the entire population is not accessible. For
example, if sample is to be taken from a loaded truck, but the sample is not a representative
of the entire population.
Quota sampling is the division of a lot into groups representing various categories, and
samples are then taken from each group. 10
 Food Sampling Technique
Requirements of Good Sampling Methods
Samples are useful for their intended purpose when they are taken in a manner consistent
with generally recognized good sampling techniques and good sampling practices. This
requires the following:
 Inspection of the lot before sampling.
 Use of suitable sampling devices and containers to hold the sample for the particular
commodity and type of sample desired.
 Maintenance of the integrity of the sample and associated records.
 Use of adequate precautions in preserving, packing and delivery of the sample to the lab
in a timely manner.
 Provision of appropriate storage conditions for the sample both prior to and following
analysis.
All of these factors, along with others such as cost versus benefits analysis, and a review of
program objectives and regularity requirements, are to be assessed and brought together in a
sampling plan that serves as a guide to management, as well as to operating personnel as a
firm plan to achieve quality in sampling.
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 Food Sampling Technique
If the quality characteristics
After a lot is received, a Lot Received
are satisfied, the lot is
sample of items is selected for accepted and send to the
inspection. The results of the Sample Selected
production or shipped to
inspection are compared to customers. If the lot is
Sample inspected for quality
specified quality rejected, managers must
characteristics. decide on its deposition.
Result compared with
specified quality
Quality is characteristics Quality is not
satisfactory satisfactory

Accept the Lot Reject the Lot

Send to production or to
Decide on disposition of the
customer
Lot

Fig. Acceptance Sampling Procedure

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 Food Sampling Technique
In other cases, the lot may be return to the supplier at the supplier’s expense; the extra
work and cost placed on the supplier can motivate the suppliers to provide high – quality
lots. Finally, if the rejected lot consists of finished goods, the goods must be scrapped or
rework to meet acceptable quality standard.
State of the lot
The statistical procedure of acceptance sampling
is based on hypothesis testing methodology. The
null and alternative hypotheses are stated as Ho : True HA : False
follows: Good Quality Lot Poor Quality Lot
Accept the Lot
Correct Decision Type II Error
(accepting a poor
Decision – quality lot

Reject the Lot Type I Error Correct Decision

(rejecting a good
– quality lot
Fig. Outcomes of acceptance sampling. 13
 Food Sampling Technique

Above Fig. shows the results of the hypothesis testing procedure. Note that correct
decisions correspond to accepting a good-quality lot and rejecting a poor-quality lot.
However, as with other hypothesis testing procedures, we need to be aware of the
possibilities of making a Type I error (rejecting a good-quality lot) or a Type II error
(accepting a poor-quality lot).
The probability of a Type I error creates a risk for the producer of the lot and is known
as the producer’s risk. For example, a producer's risk of 0.05 indicates a 5% chance
that a good-quality lot will be erroneously rejected. The probability of a Type II error, on
the other hand, creates a risk of the consumer of the lot and is known as consumer’s
risk. For example, a consumer’s risk of 0.10 mean a 10% chance that a poor-quality lot
will be erroneously accepted and thus used in production or shipped to the customer.
Specific values for the producer’s risk and the consumer’s risk can be controlled by the
person designing the acceptance sampling procedure/plan.

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 Food Sampling Technique
An acceptance sampling plan consists of a sample size ‘n’ and an acceptance criterion ‘c’.
The acceptance criterion is the maximum number of defective items that can be found in
the sample and still indicate an acceptable lot. It follows the binomial probability
distribution.

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 Food Sampling Technique
Q. Let us begin by assuming that a large shipment of the item x where 5% of the items are
defective. For a lot with 5% of the items defective, what is the probability that the n = 15, c = 0
sampling plan will lead us to accept the lot?
Using the above equation, f(0) will provide
For our example acceptance sampling plan, n = 15; the probability that zero item of x will be
thus, for a lot with 5% defective (p = 0.05), we have defective and the lot will be accepted. Using
the above equation (since , the probability
computation for f(0) is:

We now know that the n = 15, c = 0 sampling plan

has a 0.4633 probability of accepting a lot with 5%
defective items. Hence, there must be a
corresponding probability of rejecting a lot with
5% defective items.

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 Food Sampling Technique
Sampling plans
When materials are to be inspected by sampling there are various approaches to sampling,
such as :
a) Single sampling plan
b) Double sampling plan
c) Sequential sampling plan
Single sampling plan
In single sampling plan two number n and c should be specified in advance. The sample size n
is taken from a lot and c is the acceptance number that specifies the maximum number of
defectives that can be accepted to accept the whole lot. That is, if the number of defective
items are more than c, the entire lot is rejected or fully screened.
i. A sample of size n is selected, inspected and the number of defectives items are identified.
ii. If the number of identified defectives d, d>c, reject the whole lot
iii. If d < c, accept the lot
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 Food Sampling Technique
Double sampling plan
The double sampling plan follows the following steps:
i. A sample of size is taken and the number of defectives items are identified, if
defectives items < accept the lot and
 if > reject the lot
 If < < the another sample of size is taken
The defective items in second sample is identified
 If the lot is accepted, reject the lot otherwise

Sequential sampling plan

In sequential sampling plan a sample of lot size is taken and is identified. If the lies on the
area of rejection, the lot is rejected and if lies in the acceptance region, accept the lot.

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 Food Sampling Technique

6
i o n
je ct
5
e
(Commutive ) C
f R
a o n
e o
ati
3 4
Ar n u
nt i
o c e
f C an
o pt
re a cce
2

A f A
a o
e
Ar
1

0
10 20 30 40 50
(Commulative) n
Fig. Sequential Sampling plan
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 Food Sampling Technique

But, if the lies in between c value, it lies in the area of continuation and then another
sample of size is taken. The defective items () in sample () are compared with c. The
decision rule follow the same pattern. The lot is accepted or rejected as () lie on the area of
acceptance or are of rejection.
Another sample of the size is taken if it lies on the area of continuation
Again, () from sample () are compared with value of c, and the process continues.

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 Food Sampling Technique
The Operating Characteristics Curve (OC Curve)

In sampling plan where the inspection process is prefect, 100 percent inspection will
provide zero probability of making error. That is, the sampling plan will not accept any
sample with defective more than acceptable quality level (AQL), in case of perfect
discrimination of an inspection process.

The plot of probability of acceptance versus the

1
Prob. of accepting Lot

fraction of defectives in a lot provides a curve

called “operating characteristics curve” or
0.5

OC curve for a sampling plan.

AQL = 0.03

0
.02 .04 .06 .08 0.1
Fraction Defective in a lot
Fig. OC curve with perfect Discrimination 21
 Food Sampling Technique

Prob. of acceptance

1
Larger the sample, the curve is more
steeper when the c is at the same n = 32
proportion. With change in value of n c= 1
and c, the OC curve changes n = 200

0.5
c= 8

0
.02 .04 .06 .08 0.1
Fraction Defective in a lot
Fig. The OC curve

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 Food Sampling Technique
Producer’s Risk and Consumer ‘s
Risk
While using the sampling data, there is always risk involved.
One might reject the good lot (Type I error) or mistakenly accept the bad lot (– Type II
error). When sampling plan is adopted, the consideration of both type of risk are taken.
The AQL is the maximum percentage of defective considered satisfactory. The AQL is
usually greater than zero. The producer want a probability that lots of this quality will be
accepted. But, sometimes a lot with defectives below AQL can also be rejected and the
probability is called producer’s risk (Type I error). Since the rejection of good lot result in
high cost of production due to cost of rework, cost of wastages and other costs this
probability is called ‘producer’s risk’.
In acceptance sampling, there is some upper limit to the percentage of defective items in a
lot that a consumers willing to tolerate and beyond this level consumer will not like to
tolerate the defects. This limit is called “Lot Tolerance Percent Defective (LTPD)”. If by
mistake a lot is accepted during inspection process, where proportion of defective item is
more than LTPD, the probability is called “consumer’s risk” (Type II error).
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 Food Sampling Technique
Thus there is always trade – off between consumer’s risk and producer’s risk, finding a
sampling plan that will meet the desire s of both consumer and producer.
A combination of and AQL and and LTPS can be plotted in an OC curve. The objective is to
find a plan with an OC curve that passes through or almost through these point s AQL and
LTPD. Producer do not want to
reject the lot below AQL LTPD
Probability of acceptance

.95 1

Producer’s risk Consumers do not want items

to be accepted beyond LTPD

Many trial and error methods should be done for OC

0.5

curve to pass through points AQL and LTPD

AQL = 0.02 Consumer’s risk

0
.02 .04 .06 .08 .1 .12
Fraction Defective
Fig. OC curve Showing 24
 Food Sampling Technique
The approximate sample size mentioned in food rule 2027

SN Article of Food Approximate 14.  Jams, jellies, fruits, vegetables 300 grams
quantity (prepared, processed)
recommended 15.  Spices 200 gm
1.   Milk 250 ml 16.  Tea 125gm
2.  Ghee 150 grams 17.  Biscuits 250 grams
3.  Butter 150 grams 18.  Confectionaries 250 grams
4.  Khuwa 250 grams 19.  Salt 250 grams
5.  Curd/ (Dahi) 200 grams 20.  Food, dalahan, telahan 250 grams
6.  Baby milk food 450 grams 21.  Keshar, color etc. 150 grams
7  Baby food 450 grams 22.  Readymade processed food 250 grams
8.  Milk powder 250 grams 23.  Sugar 200 grams
9  Condensed milk 250 grams 24.  Honey 150 grams
10.  All kinds of ice-cream 300 grams 25.  Sakhar(Chaku, Gund) 200 grams
11.  Oil 250 grams or 26.  Flour (all kinds) 250 grams
225 ml 27.  Aerated water (soda lemonade 300 grams
12.  Vanaspati(vegetable) ghee 150 grams etc.)
13.  Fats (except ghee and oil) 125 grams

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