Comprehensive Grade Analysis and Discussion

Comprehensive Grade Analysis Discussion (Educational)

Grade analysis discussion

This discussion is designed to help understand the bases for quality analysis of shea butter. The certificate of analysis is not included in this document.  The document discusses and reference to the laboratory values reported in the certificate of analysis.   In this document the test sample is referred to as sample batch #1.

 

CERTIFICATE OF ANALYSIS

Presented by

The American Shea Butter Institute

 

Segments from Sample Batch # 1

Report are Discussed

 

I. INTRODUCTION

II. MICROBIOLOGICAL ANALYSIS

III. METAL CONTENT

(A). Metals

(B). Metal Content of Sample  Batch #1

(C). Source of Iron and Other Metals

(D). Water as a Major Source for Metals

IV. PEROXIDE LEVEL

Storage Conditions That Promote Peroxide Formation

Efforts to Retard or Prevent Peroxide Formation

Effect of Storage and Age on peroxide production and thus quality

Conditions for best Outcome during storage   (HALT)

Monitoring the Effectiveness of Sample  Batch #1 Storage Environment

V. FREE FATTY ACIDS

(1). Factors Known to Degrade and Destroy Shea Butter

IV. FATTY ACID PROFILE

VII. SHELF LIFE

VIII. RANCIDITY

Oxidative Rancidity

Biological Oxidative Rancidity

Metals Induced Rancidity

Hydrolytic Rancidity and High Temperatures

Oxygen and Spontaneous Decay

IX. BIOACTIVE FRACTION

X. SUMMARY

Recommended Uses for Grade D Shea Butter

I. INTRODUCTION

The information below will provide assistance in understanding the laboratory results presented in the Certificate of Analysis. The information explains the lab test results in simple, easy to understand terms. In addition, ASBI has made recommendations to help maintain and improve the quality of future productions.

This information is most valuable for the production team. The production team can improve the quality of the butter by adopting and implementing the recommendations contained within this report.

II. MICROBIOLOGICAL ANALYSIS

Microbial Contamination can be potentially harmful to the end user. The personal care industry strongly opposes the use of microbial contaminated shea butter.   The most common microbial contaminants found in unrefined shea butter are mold, yeast, and fungi. The most dangerous microbial contamination comes from the Coliform organisms, such as E.coli, Salmonella, Shigella, etc. The presence of Coliform organisms is indicative of unsanitary conditions during preparation.   Whenever coliforms are found, the entire operation must be shutdown until the source of these pathogens are identified and corrected

Any shea butter found to contain microbial contamination automatically receives a quality Grade of F.  Shea Butter with microbial contamination of any type is not recommended for use in the personal care industry.

We performed over a half of dozen tests on Sample Batch #1 in search for microbial contamination. We are pleased to report Sample Batch #1 does not contain any evidence of Coliform mold, yeast or fungal contamination.

III. METAL CONTENT

We test for metal content in shea butter for a number of reasons. Metal contamination of any kind increases free fatty acid formation, increases peroxide formation, increases rancidity, reduces shelf life, and reduces the quality grade of shea butter.  For that reason every effort must be made to reduce or prevent metal of any kind in shea butter.

(A). Metals

Heavy metals such as lead and mercury, in addition to promoting rancidity, can be potentially harmful to the health and well being of the end user. Therefore any shea butter found to contain lead or mercury automatically receives a quality grade of F, and is not recommended for use in the personal care industry.

(B). Metal Content of Sample Batch #1 Shea Butter

When we studied the metallic content of Sample Batch #1 shea butter neither lead nor mercury were found. This observation is considered excellent. When we looked for other metals we found iron at 2.0 mg per kg.  This is considered this value borderline poor.  We like to see the iron content below 2 mg/kg. The high iron content in Sample Batch #1 is a major contributes to the high peroxide of 5.61 millequivalents per kg.

(C). Source of Iron and Other Metals

To reduce iron content in shea butter make sure all utensils, pots and other instruments are made of stainless steel, or wood or plastic. The mechanical crushing and milling equipment must be stainless steel.  Check to make sure that the water used does not have high iron content.

(D). Water as a Major Source for Metals

The importance of water quality used in shea butter production is often overlooked.  Water with high metallic content will produce poor quality shea butter.  The major sources of water in communities where shea butter is made are well water, rainwater, and river water. Obviously, well water is preferred over rain or river water. Below are the most common metals found in samples of well water through out East and West Africa. The use of water containing one or more of the agents listed below will guarantee poor quality shea butter.

AluminumCalciumManganese LeadCopperZinc MagnesiumIronCadmium

 

Deionized water is the best water for production of high quality shea butter. Unfortunately, deionized water is not readily available in shea butter producing communities.  When using well water, it is strongly recommended to test water for its metallic content.  You send a sample of water for metallic analysis to ASBI lab or a lab of your choice.  If laboratory results reveal the water has a high metallic content you must identify another water source with less metal. Sometimes a good micro-filtration system can reduce metallic content.   Increasingly more and more processors are following ASBI recommendation by   performing waterless extraction and processing of shea nuts to shea butter.

(E). Proper equipment maintenance between extractions reduces metal oxides formations

The best equipment and utensils for shea butter extraction should be  made of stainless steel, plastic or wood.

Equipment and utensils made of any other material is likely to increase the metallic content of shea butter. Increased metallic content means lower quality.   Maintenance of good clean equipment also helps to reduce metal oxides formation on the surface of equipment between extractions.  To that end, when extraction is completed, all equipment, used in the extraction, must be washed with soap and water, hand dried then carefully and completely oiled down, with fresh shea butter or some other clean vegetable oil.

Between extractions, oiled equipment and utensils should be kept in a room where the temperature is controlled and maintained at 70 degree Fahrenheit or less.

When ready for the next extraction, remove the equipment and utensils from the temperature controlled room; again wash all equipment and utensils with warm soap and water then rinse several times with clean water to remove any residual oil that may have gone rancid during storage.

VI. PEROXIDE LEVEL

The peroxide level in Sample Batch #1 Shea butter was found at 5.61meq/kg.  This value is too high; the peroxide value should not exceed 2 meq per kg, (two millequivalents per kg).

On the day of extraction, the peroxide level is always zero or close to zero.  For the peroxide level to rise from zero in July of  to 5.61 meq per kg by August   suggest serious corrections must be made in one or more extraction steps or in post extraction management. The rate of peroxide formation by Sample Batch #1 is eight times faster than the preferred rate of 0.5 meq per kg. This process profoundly limits the shelf life for Sample Batch #1.

To improve the quality grade of shea butter it is important that you make every effort to identify those factors that may cause a rapid rise in peroxide.

Below are suggestions to Retard or Prevent Peroxide Formation

1.    Use only plastic, wood or stainless steel utensils and equipment during (1) fruit / nut preparation, (2) oil extraction, (3) packaging, (4) storage and (5) shipping of Shea product.

2.    All equipment, utensils, pots and bowls must be plastic, wood or stainless steel; all others are unacceptable for production of high quality shea butter.

3.    As mentioned early, metal of any type will promote peroxide formation

4.    One fundamental law in shea butter preparation is NEVER MIX NEW FRESHLY PREPARED SHEA BUTTER WITH OLD BUTTER. One bad apple spoils the barrel.

5.    Inappropriate post extraction storage environment is a major cause for peroxide formation. Once shea butter extraction is completed, make every effort to keep the butter in airtight containers stored in a dark, cool and dry area.

6.    Maintain an aseptic storage environment.

7.    Maintain aseptic practices when transferring Shea butter from one storage container to another

8.    Do not use storage and shipping containers made of materials other than stainless steel, plastic or wood.

9.    Always thoroughly wash, where possible steam clean, and thoroughly dry all storage containers prior to use. It is absolutely imperative that these containers are clean and well dried before filling with shea butter.

10. In the post extraction period, there exist certain factors that must be understood to better manage shea butter in the out months..  Under improper storage conditions, see halt below, fatty acids will react with oxygen to form peroxides. The common peroxide forming fatty acids are;

 

1). Alpha Linolenic

2). Linoleic

3). Oleic

4). Eicosenoic

5). Gamma Linolenic

 

East African shea butter has a larger content of peroxide forming acids when compared with West African shea butter. Further, East African shea butter has less antioxidant than West African shea butter.  This fact explains why East African shea butter produce peroxides faster than West African Shea Butter.

The term HALT defines the fundamental law for shea butter storage.

 

Humidity (low humidity /dry)

Air: Containers should be closed airtight.

L Light is undesirable. Shea butter should be stored in a dark area

T Storage temperature should 70 F or lower. Higher temperatures promote peroxide formation.

Effect of Storage on peroxide production and thus quality

 

All biological materials are undergoing continuous decay. This fact explains why quality is lost with age.  The decay process occurs even in the most ideal storage conditions. Decay is oxygen driven. Oxygen must be present for biological material to decay. Therefore keeping the containers sealed airtight prevents oxygen exchange, thereby reduces decay over a given period of time.

  1. Avoid opening and closing of storage containers.  Once the butter is rancid you have lost serious capital.
  1. Quality decreases as the butter ages.
  1. Properly prepared shea butter free of microbial contamination, metal contamination, and moisture contamination, properly stored in air tight container(s) in a climate controlled storage environment should hold its quality value for well over a year.

The graph below shows shea butter that was stored at various temperatures for 6 months and the peroxide content determined monthly from each temperature point.

 

The results show as the temperature increases from 70° to 90° degrees, there is a corresponding increase in the rate of peroxide formation.   The ideal storage temperature is noted as 70° F. This finding shows the preferred rate of peroxide formation is 0.25 – 0.50 meq per kg per month.

Monitoring the Effectiveness of the Storage Environment

The two parameters that give the best indication regarding optimum storage environment are FFA and peroxide.  To monitor the effectiveness of storage conditions you should obtain a monthly peroxide valve and a monthly FFA value.

(5). In an Ideal environment, for a pure, properly prepared, uncontaminated shea butter, peroxide changes should be less that 0.5 meq per kg per month, while FFA changes less than 1% per month.

If the change in peroxide is greater than 0.5 meq per month, the storage environment is inappropriate or the shea butter has serious issues such as metal contamination, microbial contamination, or other undesirables such as the improper storage containers, storage temperature maybe to high, storage containers may not be air tight. It is important to make every effort to determine the cause of a rapid rise in peroxide value during storage.

V. FREE FATTY ACIDS

The amount of free fatty acids present in a given Shea Butter tells us the degree of destruction and digestion that has occurred.  The presence of free fatty acids above 2% is indicative of significant destruction and breakdown of important ingredients, especially the Triglyceride.

For this reason the higher quality rating is awarded to those butters with the free fatty acids below 2 %. During quality evaluation, the highest possible score a given shea butter can earn is a total of 139 quality points. The FFA contribution to the 139 quality points can be as much as  25 points. Those butters with a FFA of 2% or less are awarded the maximum of 25points. Butters with FFA of 6% or greater are awarded only 5 points.  That shea butter with FFA between 2% and 6% are awarded a point value between 25 and 5 points.  The FFA contribution in Sample Batch #1 was found to be 4.17 %, which is considered poor.

Free Fatty Acid

Lab value

Rating lab value

Quality Points awarded

based on  FFA value

 

0 – 2 %

Excellent

25 points

 

2 – 4 %

Good

Omitted here

 

4 – 6 %

Fair

Omitted here

 
 Greater than 6 %

Poor

5 points

 

 

 

Destruction of the natural integrity of Shea Butter to liberate FFA

There are several parameters known to increase Free Fatty Acids.  These conditions occur in each of the three phases of extraction, namely:

  • The pre – extraction phase
  • The heating/cooking phase of extraction
  • The post extraction phase

(A). Pre extraction phase: Prolonged digestion time is the major pre-extraction contributor to elevated FFA.

In the traditional extract method the time period between the crushing-milling step and heating step is referred to as the DIGESTION TIME. .

  • Care must be taken to avoid a prolonged DIGESTION TIME.
  • The ideal DIGESTION TIME is 0 -1 hour.
  • Never allow milled paste to sit overnight.
  • Prolonged digestion time results in marked increase in FFA
  • When an oilseed cell is ruptured during crushing-milling step a large pool of digestive enzymes is released.
  • These enzymes digest valuable ingredients in the oil.
  • This digestion is optimal at temperature range 30 – 60° C.
  • Temperatures above 60° C inactivate the digestive enzymes.
  • The inactivation temperature is achieved during heating step.

This information should help you understand why the digestion time (defined earlier) is a quality-determining step.

The digestive enzymes mentioned above are cited below.

Enzyme

Substance Digested

Digestion product

Lipase

Triglycerides

Free Fatty acids

Protease

Protein

Amino acids

Amylase

Complex sugar

Simple sugars

DNAase

DNA

Nucleic  acids

RNAase

RNA

Nucleic  acids

(B). Factors that increase Free Fatty acids during Heating/Cooking phase:

  • Prolong digestion time results in increased FFA content.
  • Inappropriate heating temperature i.e., too high; or too low. Ideal heating temperature is 90° C,
  • Using hard water for processing. Hard water has a higher metal content. Metals serve as catalyst and increase rate of triglyceride destruction therefore increasing FFA content

(C). Factors that increase Free Fatty acids in the Post extraction phase:

 

  • Storage temperature above 70° F
  • Moisture content, greater than 1%
  • Storage containers opened to air,
  • Storage containers exposed to sunlight.
  • Microbial contamination

 

VI. FATTY ACID PROFILE

The fatty acid profile for Sample Batch #1 is within acceptable limits. The Oleic acid / Stearic acid ratio was within normal limits for East African shea butter. . The Palmitic acid/ Oleic acid ratio was within normal limits. To that end, there was no indication for Triglyceride profile; therefore, test performed

 

Sample Stearic / Oleic

Ratio

Oleic / Palmitic Ratio

32.04   / 55.49

=  0.557

55.49 / 3.93 14.12

 

VII. SHELF LIFE

Shelf life is considered the amount of time before a given shea butter is rancid.

We consider a shea butter is rancid once the peroxide level reaches 6-meq/per kg.  The amount of time required for a given shea butter to go rancid is dependent on a number of intrinsic and extrinsic factors. Extrinsic factors responsible for rancidity are discussed in details below. Each batch of unrefined shea butter has its own unique rate of peroxide formation and thus, its own unique shelf life.

Once extraction is completed, the intrinsic factors that promote rancidity are listed below.

Moisture content

 

Metal content

Insoluble debris

Peroxide contentFree fatty acid content                                           

Light expose

Vitamin A contentVitamin E content

Storage temperature

 

The stoichiometric relation of these factors is still unclear.  However, it is clear that each of these variables plays a significant role in the butter’s shelf life.  Because the contribution of each intrinsic factor varies within each batch, it follows that the shelf life is unique for each batch.

It is profoundly incorrect to consider the shelf life for one batch shea butter the same for all shea butters.

The peroxide value is commonly zero or close to zero the day extraction is completed.  Shea butter properly prepared and maintained as recommended will require more than one year from the day of extraction to reach a peroxide value of 6 meq per kg. This rate is less than 0.5 meq per kg per month.  The rate at which peroxide in any shea butter goes from zero to 6 meq per kg is determined by the contribution of a host of intrinsic factors mentioned.

In many communities where shea butter is prepared, the physical facilities necessary to properly maintain shea in an ideal post extraction environment are not readily available. To that end, once production is completed, we strongly recommend the buyer make every effort to have the butter shipped immediately to international facilities capable of ideal post extraction management.

We recommend producers process shea butter based on new orders. Where possible, the producer should first find a buyer, and then prepare the product. Avoid preparing large volumes of shea butter before identifying a buyer.

Finally we strongly encourage shipping shea butter in refrigerated trucks and/or containers to avoid exposed to heat and other undesirable environmental factors during transport. These recommendations ensure the buyer a longer shelf life before rancidity.

VIII. RANCIDITY Factor is used to assess quality and shelf life.   Rancidity factor consists of several parameters that negatively impact the quality of shea butter. These factors are moisture, peroxide, FFA, iron, and debris. The higher the Rancidity factor the lower is the quality and shelf life

Biological products undergo continuous auto oxidation and decay.  To that end, the decay and degradation of shea butter begin as soon as extraction is completed.  Studies here at ASBI have revealed that the rancidity factor is the best predictor of shelf life for unrefined shea butter. Shea butter with rancidity factor of less than ten has a shelf life greater than one year, while those batches with rancidity value greater than 10 have a shelf life of less than one year. The rancidity factor for the Sample Batch #1 found to be 10.46.  This is a borderline value, and suggests Sample Batch #1 has a shelf life less than one year.  The same is concluded using the peroxide production rate to calculate shelf life. In reality, this butter has a limited shelf life. In 4 – 6 months the peroxide level will exceed 6 meq per kg

The # 1 Problem in Post Extraction Management of Shea Butter

Rancidity is defined as a peroxide value greater than -6 meq per kg
What causes rancidity in Shea Butter?

Unpleasant flavors and odors may develop in Shea Butter as a result of oxidative rancidity. Peroxide formation is one of the major contributors to rancidity.

This oxidative rancidity process occurs via several pathways. For the benefit of the  production team each pathway is discussed below.  Attention to one or more of these pathways can result is peroxide reduction.

Oxidative Rancidity

This is due to the oxidation of the peroxide producing fatty acids. Oxidative rancidity takes place when oxygen molecules join with the double bond of peroxide producing fatty acids and break the molecule open. As a result a variety of compounds are formed, which gives rise to off-odors and off-flavors.  Oxidative rancidity is accelerated by heat, light, and traces of metals, such as copper and iron.

Biological Oxidative Rancidity

Microorganisms (such as bacteria, mold and fungus etc.) produce certain enzymes (oxidizing enzymes) and promote oxidative rancidity in Shea Butter.  In the presence of oxidizing enzymes produced by   bacteria, mold, yeast, and other microorganisms peroxide producing fatty acids  will undergo oxidative changes to produce peroxide thereby resulting in rancid shea butter

Metals Induced Rancidity

Certain metals promote the onset of rancidity. Some metals are more effective in promoting rancidity than others. If rust is present on equipment used to process or store Shea Butter, this rust will cause a marked increase in peroxide formation.  Only a small amount of the metal is needed to form large amounts of peroxide. Therefore, the use of metal equipment to process or store Shea Butter promotes oxidative rancidity. In the future, those who prepare Shea Butter will use deionized water to reduce or eliminate impact water born metals.

Hydrolytic Rancidity and High Temperatures

Hydrolytic Rancidity results when Shea Butter is stored for prolonged periods in high temperatures. Heat provides increased energy for reactivity and promotes all forms of oxidative rancidity. This is frequently a problem at storage facilities.

It is absolutely mandatory to store shea butter in a temperature-controlled warehouse. This will reduce all other forms of rancidity. When shipping oversees for the personal care market, use only refrigerated containers.

Oxygen and Spontaneous Decay

Oxygen can also cause deterioration of Shea Butter spontaneously by itself (in such cases no metal or microorganisms required). This process is very slow and is called auto oxidation. Auto oxidation is the chief cause of quality loss in well-prepared and well-stored shea butter. This explains why Shea Butter that is stored in open containers is at a greater risk than those that are sealed airtight.

IX. BIOACTIVE FRACTION

Bioactive fraction, formerly called the Nonsaponifiable fraction, or the healing fraction. In the great majority of oils derived from fruits, vegetables and nuts the bioactive fraction is very small, often in the range of 1% or less (see chart on next page).   However, the bioactive fraction in a good preparation of shea butter can be as high as 4 -6% or greater.

It is this exceptionally large bioactive fraction that separates and distinguishes shea butter from all other oils.  Likewise, it is this exceptionally large bioactive fraction that makes shea butter superior to petroleum derived skin care products such as baby oil, mineral oil, and petroleum jelly, etc

Petroleum based oils such as mineral oil, baby oil, petroleum jelly, etc., have absolutely no bioactive ingredients.

It is important to understand that the bioactive fraction has healing ingredients for various skin ailments The size of the bioactive fraction is one of the parameters used to determine grade. Those butters with larger bioactive fraction earn a higher grade.

The size of the bioactive fraction is extremely valuable for shea butter used in the personal care industry. The larger the bioactive fraction, the more valuable the butter for personal care uses.

For any shea butter to qualify as Premium Grade A Shea Butter, the bioactive fraction must be 4 – 6% or greater for West African shea butter, and 3 – 4% or greater for East African shea butter. .     

When we studied the bioactive fraction in Sample Batch # 1 we found it was low at only 1.78% of the shea butter.  This is considered poor. Something has happened to, or with this shea butter, causing the butter to have such a smaller bioactive fraction.

The Size of The Bioactive Fraction For Various Oil

 

Oil

Size Range

 

 

 

Baby Oil

0.00–0.00%

 

 

Mineral Oil

0.00–0.00%

 

 

Olive Oil

0.6  –1.5 %

 

 

Sesame Oil

1.0  –1.5 %

 

 

Soy Oil

0.5  –1.5 %

 

 

Maize Germ Oil

0.8  –2.9 %

 

 

Refined Shea Butter

1.0–2.2 %

 

 

Argan oil

1.5 –3.5 %

 

 

Avocado

2.0 –6.0 %

 

 

Low quality Unrefined

3.0–9.0%

 

 

Sample  Batch #1

1.78%

 

 

Wheat Germ Oil

3.5 –4.7%

 

 

Higher quality Unrefined

4.0–9.0%

 

 

Certified Premium Grade A

5.0 – 9.0%

 

Our efforts to identify causes for small bioactive fraction were unsuccessful.

Some possible causes you might consider are;

  1. Use of a significant number of nuts from immature fruits
  2. Consumption of bioactive ingredients during preparation.
  3. Extraction temperature too high
  4. Extensive post-extraction manipulations to reduce impurities
  5. Heating/cooking time too long
  6. Improper storage temperature
  7. Digestion time Too long

X. SUMMARY

The quality Grade for this Shea Butter is Grade (C)

Summary of major problems

Comments

1.    Small bioactive fraction Poor
2.    Elevated peroxide level Poor
3.    Elevated rancidity value Poor
4.    Reduced Shelf Life Poor