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  1. Laboratory Methods (Food)

MPM: V-8. Spices, Condiments, Flavors, and Crude Drugs

Macroanalytical Procedures Manual (MPM) Main Page


  1. General Method for Spices, Herbs, and Botanicals
  2. Supplemental Method for Black and White Pepper
  3. Supplemental Method for Nutmegs

A. General Method for Spices, Herbs, and Botanicals (V-32)

(1) Scope

This method covers several procedures applicable to spices, herbs, and botanicals that consist of dried plant parts which have been processed and marketed in various sizes and forms. Included in this group are parts of plants such as dried leaves, seeds, fruits, bark, roots, stems, buds, and flowers. Examples of plant part(s) products include but are not limited to:

  • Leaves
    • Sage (Salvia officinalis L.)
    • Bay leaves (Lauris nobilis L.)
  • Seeds
    • Flax (Linum usitatissium L.)
    • Nutmeg (Myristica fragrans Houtt.)
    • Fenugreek (Trigonella foenum-graecum L.)
  • Fruits
    • Cardamom Elettaria cardamomum (L.) Matonâ
    • Pepper (Piper nigrum L.)
    • Paprika (Capsicum annuum L.)
    • Cassia buds (Cinnamomum spp.)
  • Bark
    • Cinnamon (Cinnamomum spp.)
    • Sassafras Sassafras variifolium (Salisb.) Ktze.â
    • Soapbark (Quillaja saponaria Mol.)
  • Roots
    • Licorice (Glycyrrhiza glabra L.)
    • Chicory (Cichorium intybus L.)
    • Comfrey (Symphytum officinale L.)
  • Rhizomes
    • Ginger (Zingiber officinale Roscoe)
    • Calamus (Acorus calamus L.)
    • Turmeric (Curcuma domestica Val.)
  • Flower Buds -- Clove (Syzygium aromaticum (L.) Merr. & Perry)
  • Flower parts -- Saffron (Crocus sativus L.).
  • Flowers -- German chamomile (Matricaria chamomilla L.)
  1. General Method -- Procedures applicable to macroscopic examination of most of these products fall into two categories:

    1. (i) A procedure for separating, identifying, and recording amounts of contaminants such as insects, animal excrement, and extraneous matter which have been removed by pick-out or mechanical means from the product material itself.
    2. (ii) A procedure for separating and classifying defective product materials (such as insect-damaged or moldy material); these are recorded as percentages of reject material by weight or count of each type of reject.
  2. Specific methods -- Procedures for certain types of products (e.g., black pepper, nutmegs, etc.) are specialized for dealing with specific problems. Special techniques related to these products are covered by supplemental methods described in Sections 8.B and C.

(2) Applicable Documents

  1. CPG 7109 Defect Action Levels
  2. 21 CFR Standards of Identity and Quality
  3. I0M 624.11 Establishment Inspection, and 624.12, Sample Collection
  4. Service and Regulatory Announcements, Food and Drug, No. 2, Nov. 1936, pp. 11-14 -- "Advisory Standards for Spices"

(3) Defects

Defects in these products may be categorized as due to insect infestation, contamination by animals, mold development, or contamination by extraneous material.

  1. Insect Infestation and Damage -- Products may be contaminated and damaged by insects in the growing area during production and harvest. Typical field insect pests include Lepidoptera, Coleoptera, Hymenoptera, Homoptera and Hemiptera. A wide variety of stored-product insects, principally Lepidoptera and Coleoptera, also attack these products. Other arthropod pests, such as mites, ticks, and spiders, may be present. Examples of insect infestation and damage range from excreta, webbing and frass, insect tunnels or evidence of surface feeding, to whole insects in the product. Although numerous insect species are associated with these products, serious damage to particular products is usually due to a few species, and it may be helpful, in some cases, to define such damage as part of a specific method.
  2. Animal Contamination -- Contamination of these products by animals usually results from either gnawing or defilement by excreta. Whole rodent pellets, bird droppings, and other pieces of animal dung are typically found.
  3. Moldiness and Fungal Deterioration -- Products may be attacked by fungi in the field or while in storage. Field fungi capable of attacking and infecting the growing product may cause varying degrees of decomposition and damage. The damage from invading fungi and molds may be manifested as leaf spot diseases, dry rot, decomposed and discolored tissue of stems and roots, or decay in seeds and fruits. Storage fungi (which can grow under limited moisture conditions) may cause moldiness in some products stored under conditions of temperature and relative humidity favorable to their growth. Pockets of moist product can arise in a dried and otherwise normal product through roof leaks, insect activity, and moisture translocation when temperature gradients develop within the product mass. These pockets can promote the rapid growth of molds in the stored product. Moldiness can range in appearance from mycelium-matted leafy spices and surface mold on cassia bark, to internal molds in nutmegs and capsicum pods.
  4. Contamination by Extraneous Material -- Objectionable matter such as sticks, stones, burlap bagging, or cigarette butts may enter the product at various points during its production, transit, and storage because of improper preparation or handling. Also, valueless parts of the raw plant material and other foreign plant material may contaminate the product and require special attention for removal. This general category is intended to include all other miscellaneous objectionable matter not reported in the other specific categories.

(4) Procedure: Determination of Contamination in Spices, Herbs, and Botanicals Caused by Insects, Animal Excreta, and Extraneous Material

  1. Sample Preparation -- Sample a representative or selective number of analytical units of the lot sample, depending on the history of the lot.
  2. Visual Examination -- Analyze 300-500g subsamples of high density products (cassia, ginger, cloves, allspice, turmeric, condimental seeds) and 200-300g subsamples of light, bulky products (capsicum pods, mace, leafy spices). Examine the product in small amounts with good light and against a white or other suitable contrasting background. A moving belt or other mechanical device may be used if all the material can be seen easily. Sifting may facilitate separation and concentration of certain types of objectionable matter. Examine macroscopically for rodent excreta, manure, insects, and insect debris, mold clumps, miscellaneous objectionable matter, and other evidence of contamination. If sifting is performed, size of screens used and method of use should be stated in the report of results.
  3. Classification of Contaminants -- Separate contaminants into suitable groupings relative to defect action levels, regulatory guidelines, or other applicable requirements. Add categories to tabulation of results depending on type(s) of contaminants found. Classify as follows:

    1. (i) Insects -- Count number of whole insects and equivalent visible to the naked eye (corrected as necessary for abnormal vision) with such magnification as may be necessary. If the magnification exceeds 10X, this should be stated in the report of results. Identify insects, using appropriate insect identification keys. Classify insects as "Field" or "Storage," making a special notation when they are found alive. Note the size of any unidentified insects and larvae found.
    2. (ii) Rodent (Rat or Mouse) Excreta -- Rodent excreta pellets are normally black or dark colored, roughly cylindrical, blunt at one end and pointed at the other. They range in length from 1.5 to 15 mm. They usually contain rat or mouse hairs, partially digested plant material, and sometimes insect parts. When wet with water, rodent pellets form a characteristic gray mucous coating. Weigh suspect pellets and report as such only if rat or mouse hairs are present. Confirm identification by removing a hair from the pellet and identifying it microscopically. When none are present, proceed with AOAC 44.B08-44.B11, alkaline phosphatase method for mammalian excreta.
    3. (iii) Animal Dung -- Animal dung consists of an amorphous, usually dark colored material pressed into a matrix. Incorporated plant material usually consists of ligneous, fibrous material which is either pale-yellow or green. Parts of insects and small amounts of inorganic, earthy material may also be present. Weigh suspect material and report as animal dung or excreta, only when matricized plant material predominates. Confirm as excreta, using 44.B08-44.B11, alkaline phosphatase method for mammalian excreta.
    4. (iv) Bird Excreta -- Bird excreta will appear as rounded droppings, sometimes coiled with a white residue. Weigh droppings and test a portion of the white, amorphous particles for uric acid by AOAC 44.177 or 44.183 - 44.185.
  4. Report -- Tabulate results as follows, adding additional categories as necessary:
      Subsample No.
    1 2 3 etc.
    Weight Examined (g)        
    Excreta (mg/lb)a        
    Whole Insects or Equivalentb        
    Extraneous Material (% by wt)c        
    a Excluding insect excreta
    b Describe ((4)c(i))
    c Describe ((3)d)
    d Substitute appropriate heading(s)

(5) Procedure: Determination of Insect-Damaged, Moldy, and Otherwise Reject Product Material in Spices, Herbs, and Botanicals

  1. Sample Preparation -- Weigh or count out representative analytical units from sieved material remaining after completing procedure (4). Alternatively, draw analytical unit directly from sample. Prepare a composite analytical unit, if appropriate, taking an approximately equal weight of product from each subsample. State how analytical unit is taken. AOAC methods are available for light filth in leafy products and excreta in condimental seeds.
  2. Visual Examination -- Examine each product piece in the analytical unit for reject material visible to the naked eye. Magnification may be used for confirmation, as necessary. If the magnification exceeds 10X, this should be stated in the report of results. Classify, weigh, or count each category according to (5)c. below.
  3. Classification of Reject Product Material -- Classify reject product material (leaf, seed, fruit, root, bark, etc.) as follows:

    1. (i) Insect-Damaged -- Any product material exhibiting definite evidence of insect feeding or containing one or more whole insects or equivalent, webbing, or excreta. Determine, if possible, whether infestation is "Field" or "Storage," making special notation for live insects. Determine average length and note range of lengths for any larvae and/or unidentified insects present. Examine 50 g subsamples of bay leaves for field insect damage according to instructions given in Figure V-12.
    2. (ii) Moldy -- Any product material bearing mold on more than 1/4 of its surface area or any material where the aggregate moldy area is greater than 1 cm2. Confirm presence of mold with magnification as necessary, but determine the area affected without magnification. Describe general appearance of the moldy areas.
    3. (iii) Animal-Contaminated -- Any product material showing animal excreta, animal chewing, or gnawing.
    4. (iv) Otherwise Reject Material -- Any product material that is not classified as above, but is otherwise decomposed, discolored, abnormal in appearance or otherwise unfit for food.
  4. Report - Tabulate results as follows:
      Subsample No.
    1 2 3 etc.
    Amount Examined
    (wt or no. of units)
    Wt or No.
    Wt or No.
    Animal Contamination
    Wt or No.
    Total Percent of Reject        
    a Describe ((5)c.(i)); report under Remarks
    b Describe ((5)c.(ii)); report under Remarks

B. Supplemental Method for Black and White Pepper (V-39)

(1) Scope

This method supplements and/or replaces those procedures in Section 8.A., by describing procedures specific to black and white pepper (Piper nigrum (L.). The term "siftings and pickings" is used to describe certain objectionable matter which may be present in black and white pepper. When examining black or white pepper, the procedure for "siftings and pickings" described below may be used in lieu of Procedure (4), Section 8.A.

(2) Applicable Documents

  1. CPG 7109.17 Defect Action Levels

(3) Procedure: Determination of "Siftings and Pickings" and Animal Contamination in Pepper Berries

  1. Special Apparatus -- This procedure calls for use of a standard pepper sieve. The sieve consists of a No. 9-1/2 round screen with a frame 18 to 22 in. in diameter and 2-3/4 in. in height. The bottom is a metal sheet perforated with round holes 7/64 in. in diameter with an average of 5-1/2 holes per linear inch (small or "office" size 8-9 in. in diameter). U.S. Standard No. 8 sieves (0.0937 in. or 2.38 square mm opening) provide equivalent sieve opening. A perforated sieve, but not the finished unit, may be obtained in the U.S.A. from Beckley Perforating Company, 315 North Avenue, Garwood, NJ 07027, or from McNichols Company, 5501 gray Street, Tampa, FL 33609.
  2. Siftings -- Combine aliquots from each subsample to give a composite sample of approximately 4 kg, unless product lot variability indicates analysis of individual subsamples. Weigh composite sample and divide into approximately two equal portions. Screen each portion separately, using the standard pepper sieve (when using the small or "office" sieve, screen only 400 to 500 g at a time) or the U.S. No. 8 equivalent. Obtain the siftings by tilting the sieve from side to side so that the pepper passes from one side of the sieve to the opposite side 10 times. Weigh siftings after removal of pinheads/light berries. Examine siftings; identify, describe, and quantify, as necessary.
  3. Pickings -- After sifting, hand-pick sample ("overs" on the sieve) for foreign material such as sticks, stones, stems, clay, foreign seeds, and other extraneous matter. Weigh pickings other than animal contamination (3)d.â identify, describe, and quantify, as necessary.
  4. Animal Contamination -- Report contamination other than insect excreta separately from siftings and pickings. Examine siftings and pickings for animal contamination, such as mammalian excreta, bird excreta, and whole insects or equivalent. If appropriate, examine a separate analytical sample of approximately 500 g. Classify, weigh, and report as in (3)e.
  5. Report -- Tabulate results as follows, adding additional categories as necessary:
      Subsample No.
    1 2 3 etc.
    Weight Examined (g)        
    Mammalian Excreta (mg/lb)        
    Whole Insects or Equivalenta        
    Siftings and Pickings (percent by wt)        



    a Describe in Section 8.A.(4)a(i); report under Remarks
    b Substitute appropriate headings(s) such as bird excreta, etc.

(4) Procedure: Determination of Insect-Damaged, Moldy and Otherwise Reject Pepper Berries

Follow Procedure (5) in Section 8.A. for detection of pepper berries with external defects. Examine representative sample of 200 or more berries. Cut open any suspect berries as necessary. Examine, classify, and report as in 8.A(5)b, c, and d.

C. Supplemental Method for Nutmegs

(1) Scope

This method supplements Section 8.A., by describing procedures specific to nutmegs (Myristica fragrans Houtt.).

(2) Applicable Documents

  1. CPG 7109.16

(3) Procedure: Determination of Contamination in Nutmegs Caused by Insects, Animal Excreta, and Extraneous Material

Examine as in 8.A.(4)a-d. For whole nutmegs, use analytical sample of 500 g or more.

(4) Procedure: Determination of Insect-Damaged, Moldy, and Otherwise Reject Nutmegs

  1. Sample Preparation -- Weigh and examine at least 100 nutmegs from each subsample. Cut each nutmeg in half lengthwise with a sharp knife, pruning shears, or similar implement.
  2. Visual Examination -- Examine the cut surfaces of each nutmeg for presence of insects or signs of insect damage, presence of mold, or other evidence of defilement.
  3. Classification of Reject Material -- Classify as moldy (reject) any nutmeg showing mold on 1/4 or more of the cut surface. For other categories of rejects, classify as in Section 8.A., (5)c.(i), Insect-Damaged; (5)c.(iii), Animal-Contaminated and (5)c.(iv), Otherwise Reject Material. Weigh each category of rejects.
  4. Report -- Tabulate results as in 8.A.(5)d.


(1) American Spice Trade Assn. Inc., Cleanliness Specifications for Unprocessed Spices, Seeds and Herbs, ASTA, 580 Sylvan Ave., Englewood Cliffs, NJ 07632, Jan. 1983.

(2) ASTA, Official Analytical Methods of ASTA, 2nd Ed., 1968.

(3) Parry, J. W., Spices - Their Morphology, Histology, and Chemistry, Chemical Publishing Co., Inc., New York, NY, 1962.

(4) White, Ralph T., "Studies on the Storage and Shipment of Whole Black Pepper Grown in the Orient," J. Econ. Entomol. 50: 423-428, 1957.

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