chapter Analysis for Extraneous Matter Hulya Dogan,* Bhadriraju Subramanyam, and John R. Pedersen Department of Grain Science and Industry, Kansas State University, Manhattan, KS 66506, USA degan@k-state.edu sbhadrir@k-state.edu \ 19.1 Introduction 19.2.1.4 Light Filth 35: 19.1.1 Federal Food, Drug, and Cosmetic 19.2.1.5 Sieved Filth 354 Act 353 19.2.2 Diagnostie Characteristics of Filth 354 19.1.2 Good Manufacturing Practices 353 19.3 Official and Approved Methods 254 19.1.3 Defect Action Levels 953, 19.4 Basic Analysis 355 19.1.4 Purposes of Analyses 353, 19.4.1 Sieving Method 355 19.2 General Considerations 253 19.4.2 Sedimentation Method 356 19.2.1 Detinition of Terms 363 19.4.3 Flotation Methods 356 19.2.1.1 Extraneous Materials 354 19.4.3.1 Cracking Flotation Method 357 19.2.2.2 Filth 954 19.4.3.2 Light Fith Floatation 19.2.1.3 Heavy Filth 935 Method 357 5, Nielsen, Food Analysis, Food Science 14419-1478-1.2, 381 © Springer Science -Buisiaess Media, LUC352 Partill © Chemical Properties and Characteristics of Foods 19.4.4 Opjectivity/Subjectivity of Methods 358 19.5.8 Enzyme-Linked Immunosorbent | 19.5 Other Techniques 358 Assays 361 125.1 Overview 358 19.6 Comparison of Methods 361 19.5.2 X-Ray Radiography 197 Isolation Principles Applied to Food 19.5.3 X-Ray Microlornography 359 Processing 363 19.5.4 Electrical Conductance Metrod 360 19.8 Summary 19.5.5 Impact-Acoustic Emission 360 19.9 Study Questions 364 19.5.6 Microscopy Techniques 360 19.10 Acknowledgement 364 19.5.7 Near-Infrared Spectroscopy 361 19.11 Relerences 264Chapter 19 + Analysis or Extaneous Matar 363 19.1 INTRODUCTION Analysis for extraneous matter is an important ele- ment both in the selection of raw materials for food manufacturing and for monitoring the quality of pro- cessed foods. The presence of extraneous material in a food product is unappealing and can pose a serious health hazard to the consumer. It also represents lack of good manufacturing practices and sanitary con: ditions in production, storage, or distribution. The presence of extraneous materials in tae product ingre dients may render the final product adulterated and not suitable for human food. 19.1.1 Federal Food, Drug, and Cosmetic Act The Federal Food, Drug, and Cosmetic Act (FD&C Act) of 1938 with Amendments administered and enforced by the US Faod and Drug Administration (FDA) (1) defines a food as ad in whole or in part of any filthy, putrid, or decom- posed substance, or if it is otherwise unfit for food {Section 402 [21 USC 342] (a)3)] or if has been pre- pared, packed, or held under unsanitary conditions whereby it may have become contaminated with filth, or whoreby it may have been health” (Section 402 [21 (a)(4)}. The filthy, putrid, or decomposes substances referred to in the law include the extraneous matter addressed in this chapter. Jn addition, extrancous matter includes adul terants that may be encountered in processing sys tems, such as lubricants, m taminants (animate or inanimate) that may be intco- duced into a food intentionally or because of a poorly operated food processing systemn, These aspects are not covered in this chapter. ullerated “if # consists endeted injurious to al particles, or other cor 19.1.2 Good Manufacturing Practices The Current Good Manofacturing Practice in Manu- facturing, Packing, or Holding Human Food (GMFs) ublished in 1969 by the Food and Drug Admin ion (FDA) (21 CFR Part 110) to provide guid ance for compliance with the FD&C Act (2) (see also Chap. 2). That regulation provides guidelines for oper- ating a food processing facility in compliance with Section 402 (a)(4), and these guidelines have not been revised since 1986. Currently, the GMPs aze being amended to make the compliance guidelines «ore risk-based. Paramount to complying with the FDS Act and cGMPs is the thorough inspection of raw materials and routine monitoring of food process- ing operations to ensure protection of the consuming. public from harmful or flthy food proxtucts 19.1.3 Defect Action Levels Most of our foods are made from ot consist in. part o ingredients that are obtained from plants or animals and are mechanically stored, handled, and transported in large quantities. It would be virtually impossible ose materials completely free of various recognition of that, the FDA (3) has established defect action levels (DALs) that reflect curront maximum levels for natural or unavoid able defects in food for human use that present no health hazard, They reflect the maximum levels that are considered unavoidable under good manufac ing practices and apply mainly to contaminant are unavoidably carried over fro comidities into the food processing system. ‘The manser in which foods are manufactured may lead to their contamination with extraneoxs materials if strict controls in processing are not maintained, This la type of contamination leads to food safety issues, and DALs are not used to determine compliance. “ther sionable levels of contaminants may be found in the EDA Compliance Policy Guide (CPG) Manual (4). The most current information of FDA laws and regulations relevant to extraneous matter, including cGMP, DALs, and CPCs, can be found on the Inter Federal Food, Drug, and Cosmetic Act (FD&C Act hittp:/ /www.éda.gov /opacom/laws /fdcact/ fdctoc-htm Current Good Manufacturing Practices (CGMPs) ~ lattp://www.gmplstcom/tdreg him Food Defect Action Levels (DALs) ~ htty://www. an.éda.gov /~dms/dalbook html Compliance Policy Guidance (CPG) — http://www. fda. gov /ora/compliance rei/cpg, m raw agricultural 19.1.4 Purposes of Analyses The major purposes for conducting analyses for extra neous matter in foods are to ensure the protection of the consuming public from harmiul ox filthy food products, to meet regulatory requirements of the FD&C Act Sections 402 (a)(3) and 402 (a4), and to comply with DAL. 19.2 GENERAL CONSIDERATIONS 19.2.1 Definition of Terms ‘Terms used by AOAC International (AOAC Method 70.66) to classify or characterize various types of defined as follows,358 Parti * Chemis! Proper 1d Charaetanstes of Foods 19.2.1.1. Extraneous Materials Any foreign matter in product associated with obje tionable con or distribution; include tions or practices in production, storage, ave various classes of fil decomposed material (decayed tissues due to para sitic or nonparasitic causes), and miscellaneous matter such as sand and soil, glass, rust substances. Bacterial counts are not included or other foreign 19.2.1.2 Filth Aay objectionable matter contributed tamination s uch as rodent, insect, or bird matter, or any other objectionable matter contributed by unsani- tary conditions, 19.2.1.3 Heavy Filth Heavier material separated from products by sedi- mentation based on different densities of filth, food particles, and immersion liquids. Examples of such filth are sand, and pellet fragments, oil, insect and rodent excreta pellets snd some animal excreta pellets. 19.2.1.4 Light Filth filth particles that are oleophilic and are sep: rated {rom product by floating them in an oil-aqueous liquid mixture. Examples are insect fragments, whole insects, rodent hairs and fragments, andl feather bai bules 19.2.1.5 Sieved Filth Filth particles of specific size ranges separated quan titatively from product by use of selected sieve mesh sizes, 19.2.2 Diagnostic Characteristics of Filth ‘There are certain qualities characteristic to extraneous terials that serve as proof of presence of foreign or objectionable matter in food. Examples include spe cific diagnostic characteristics of malds (ie, parallel hyphal walls, septation, granular appearance of cell contents, branching, of hyphae, blunt ends of hyphal filaments, nontefracted appearance of hyphae); diag nostic characteristics of insect fragments (ie., recog nizable shape, form, or surface sculpture, an articula tion or joint, setoc or setal pits, sutures), rodent hairs (Ge,, pigment patterns and structural features), feather barbies (ie,, structural features); diagnostic charac- teristics of insectdamaged grains (IDK) and packag: ing materials; and chemical identification of animat urine and excrement. These diagnostic characteristics are outlined by AOAC International (formerly Asso- ciation of Official Analytical Chemists) for positive identification of extraneous matter or filth (5) The AACC International (formerly American Association of Cereal Chemists) publishes a methods book that includes a section on ter, containing descriptive material helpful in identifying insect and rodent contaminants (6). Several micro scopic and radiographic illust the AACC International as authentic reference mate rials to help analysts to identify filth. AACC Method 28-95, "Insect, Rodent Hair, and Radiographic Illus trations,” provides a series of colored pictures rep resentative of insect fragments commonly found in cereal products and pictorial examples of rodent hair Kurtz and Hartis (7) provide a virtual parts cata log of insect fragments with a series of micrographs. Gentry et al. (8), an updated version of the Kurtz and Harris publication, includes colored micrographs ‘of common insect fragments. Also included in AACC 28-95 are radiographic cxamples of grain kernels that contain internal insect infestation. AACC Method yy Examination for Internal Insect Inf provides an outline of the apparatus and ations are provided by tation, procedure for infestation in grain (9 ray examination of internal insect 19.3 OFFICIAL AND APPROVED METHODS There are various laboratory methods for separating (isolating) extraneous materials from foods and for identifying and enumerating then. The FDA and the AOAC International have published books, and methods on analysis of extraneous materi als, The most authoritative source, and that generally considered official by the FDA, is the Official Methods AOAC International, Chap. 16, “Extra- neous Materials: Isolation” (5). This chapter includes methods for extraneous matter isolation in various ies (Table 19-1). The AOAC International ‘Extraneous Materials: Isolation” chapter contains uubchapter dealing with molds. This includes identifi cation of moles and methods for isolation of molds in table jood cal fruits and fruit products and vegetables and vey oroducts. The ods for isolating and identifying extraneous matter in cereal grains and their products (AACC Method 28 00, listed in Table 19-2), In most instances, the AAC methods are based on FDA or AOAC methods, but the format is slightly different. The ACC presents each procedure in an outline form that includes the scope, apparatus, and reagents required and the procedure in itemized steps while the AOAC uses a narrative h form (Table 19-2), ACK International (6) has established meth:Officiat Methods of AOAC Intemational for Analysis of Extraneous Materials 6 Extraneous materials: isolation 161 General 162 Beverages and beverage materials 163 Dairy products 164 Nuts and nat products 165 Grains and their products 68 167 Breakfast cereals 168 Eggs and egg products 169 Poultry, meat, and fish and other marine Products 16.10 Fruits and fruit products 1811 ck food products 1612 Sugars and sugar products 16.13 Vegetables and vegetabie products 16.14 Spices and ether condiments 1645 Miscellaneous 16.16 Animal excretions 1647 Mole i818 Fruits ang fruit products 619 Vegetables and vegetable products, A valuable resource on analysis fo matter is Principles of Food Analysi sition and Forcign Matter, FDA Technical Bulletin No. 1 10). The FDA Training Manual for Analytical Entomet ogy iit the Food Industry (11) is prepared to facilitate the orientation of food analysts to the basic tech- niques they will need for filth analysis. A recent, more anced resource is Fundamentals of Microanalgtical Entomolagy: A Practiaa! Guide to Detecting and Identi fi Foods (12), Most chapter authors of this nel “involved piecing together the etiolog resource are, or have been, FDA perso in the fore ical puzzles of how insect filth gets into processed food products (12). The authors share their expe- rience gained in gathering and developing evidence used to document violations of the law that the FDA. is mandated to enforce, aspect of 19.4 BASIC ANALYSIS Various methods for isolation of extraneous matter are suggested in Sect, 19.3, which define different types. of filth: separation on the basis of differences in den- sity, affinity for oleophitic solvents, panicle size; diagnostic characteristics for identification of filth; and chemical identification of contaminants. Since al methods of analysis for extraneous matt gories of food cannot be di sd in this chapter, only the underlying principles of the methods are surnma rized below. Readers may need to refer to the specilic AOAC methods lor all cate: fed for detailed instructions of the Approved Methods of the AACC Intemational for Anaiysis of Extraneous Meieriats Tile me Numi 2a taneous matter 28.01.01 Apparatus or materials for extraneous matte methods 28-02.01 —Reagenis for extraneous matter methods 2803.02 Special techniques for extraneous matter methods 28:06.01 Cinder and sand particles in farina ~ ‘counting methad 28.07.01 Cinder and san panicles in farina gravimetric method Macroscopic examination of ext Contamination in whole grains Exernal fith ang internal insect infestation in whole corn Microscopic examination of external contamination in whole grains 28:2.02 X-ray examination for internal insect infestation 28-22.02 Crackingotation test for internal insects in ‘whole grains 28-30.02 Macroscopic examination of materials hard to hydrate 28-31.02 —_Pancreatin siewng method, for insect and ‘odant fith in materials hare to hydrate Sieving method, for materials hard to hydrate 28-92.02 28.33.02 Pancreatin nonsieving method for insect and rodent fith in materials easy to hydrate 2840.01 Acid hydrolysis method for insect fragments ‘and rodent hairs — wheat-soy blend Acid hyosolysis method for extracting insect regiments and rodent hairs — light fith in wnite flour Glass plate method, for insect excreta ledine methos 98 in flour 2850.01 _Decantation method, for rodent excreta 28:51.02 Flotation methad, for insect and radert Ath 28-60.02 Tween-versene method, for insect fragments ‘and adent hairs in rye flour Detatting-roper training, and supervised practice, Another concern involves the significance of insect fragment couats (as well as particles of sand, pieces of rodent excreta tion to fragment or particle size. Fragment counts are reported on a numerical basis; they do not reflect the total contaminant biomass that is present. A small rodent hairs, etc) in rela fragment is counted the same as a large fragment. The size of the fragment may be a reflection of the process towhich a common raw material (e.g., wheat) has been subjected; a more vigorous process produces moze and smaller fragments than a loss vigorous process. The state of insects may also be « factor. Dead (dried) forms >roduce greater numbers of fragments than live forms. These factors have been of concern to food processes for some time and have prompted the search for more objective means of determining insect contamination 19,5 OTHER TECHNIQUES 19.5.1 Overview Methods described in Sect. 19.3 are directed primar- ily at routine quality control efforts to determine if the level of natural or unavoidable defects is below the defect action level. To a certain extent, those routine methods can be used to identify nants in processed foods. For example, the identifica- on of certain insect fragments can indicate infestation n han in the processing system, However, other more sophisticated techniques offer opportunities to pinpoint the nature and sousce e source of contin he raw commodity rath of ather contaminants that may exist unavoidably or terial or equipment failures, or intentional adulteration The detection of insects in stored quantitation of insect parts present in uicts represent a serious and continuing problem f the grain industry. Approved methods of detection primarily involve visual and microscopic inspection and X-ray analysis, which require trained personnel and are time-consuming, difficult to standardize, and expensive. The assays for insect contamination are preferred to be highly specifi nexpensive. Moreover, it ideally should be employ able by persons having minimal training, particularly n nonlaboratory settings such as at grain elevator and processing sites ‘There are several attempts to develop rapid and efficient methods including the use of nuclear mag- amplification, and infrared spectrometry as alternatives to presently used chem ical techniques mentioned in preceding sections. Most of these techniques are expensive and challenging due to difficulty in quantification and identification of spe cific infestations. Immunological assays, which have found widespread use in clinical diagnostic settings and also in home use, have been explored to detect insect contamination, These methods are described below as they relate to detecting an infestation due to mistakes, accidents, m fain and the fain prod: sensitive, rapid, and netic resonance, sourChapter 19 + Analysis for Exraneous Mater 359 18.5.2 X-Ray Radiography X-ray radiography is wiclely used as a test reference method (14). Grain processors use it as a means of inspecting, wheat for internal insect infestation, which js the main source of insect fragments in processed cereal products (Fig. 19-5).The existing X-ray tech- niques enable the classification of at least four stages of insect development by measuring the area occu- pied by the insect, and an accurate classification is also possible based on visible insect morphology (15) Tho use of real-time digital imaging instead of radiographs to discriminate the infested kernels signil- icantly shortened the X-ray procedures. Conventional film observations give, however, better accuracy (3% error rate) than the digital images (11.7%) for infe: tion by third-larval instars, while the error is less than 1% for both methods with a more advanced stage of larval development (16) Khamis} 19.5.3 X-Ray Microtomography X-ray microtomography (XMT) is an emerging 3-D imaging technique that operates on the same basic principles as medical computed tomography (CT) scanners, but has much higher resolution. It is very effective in characterizing various internal structural features, which are not possible with corventional 2-D imaging methods. Coswentional imaging tech: niques stich as light microscopy, scanning electron microscopy (SEM), and digital video imaging have me limitations: They are destructive in nature, as sample preparation involves cutting to expose the «1056 section to be viewed. High-resolution XMT has a wide range of applications in science and engineering for which accurate 3-D imaging of internal structuce of objects is crucial X-ray radiograph of infested wheat: (a) Lesser grain borer pupae, (b) Rice weevil pupae. (Courtesy of Moses mages of a wheat kernel at various rotation angles, - Microtomographical techniques involve tanget- ing the specimen with a polychromatic X-ray beam with high spatial coherence. The X-rays not absorbed by the specimen fall on specifically designed X-ray scintillators that produce visible light, which is then recorded by a charge-coupled device (CCD) camera. Scans are done by rotating the specimen between 2 fixed X-ray source and detector, around the axis per- pendicular to the X-ray beam, while collecting radio- graphs of the specimen at small angular increments in the range 0-360", The radiographs are reconstructed into a series of 2-D slices. The series of 2-D slices are then reconstructed into a 3-D image. The resulting XMT data can be visualized by 3-D rendering or 2- D slices derived from virtual model, using software that allows reconstruction of cross sections at various depth increments and along any desired orientation of the plane of cut (17). XMTis able to capture several fea tures of the internal structures of grain kernels, which are not possible with the conventional imaging meth ods. Figure 19-6 is demonstration of shadow images360 Part ll © Chemica Properties and Char rite of Foods X-ray microtomography (XMT) images: (a) shadow image, (b) sagittal view, (e) axial view, and (@) coronal view of lesser grain borer ina wheat kernel taken at several step an, cal scan creates 200-400 of thase images that are then sed to create axial, sagittal, and coronal views shown in Fig. 19-7. during scanning. A typi 19.5.4 Electrical Conductance Method ‘The electrical conductance method is based on mor itoring the conductance signals for each single ker- nel during milling in a Single Kernel Characteristics System (SKCS), which is commonly used for wheat hardness determination (15). This method is highly accurate for detecting older developmental stages of insects: the percentage of properly classified cases for small, medium, and large larvae and pupae is 245, 622, 87.5, and 88.6, respectively. The accuracy of this method depends also on insect species (rice weevil anc lesser grain borer) and wheat type (Soft or hard ted winter wheat) 19.5.5 Impact-Acoustic Emission Impact-acoustic emissions are used as a nondestruc: tive, real-time method for detection of damaged grains and shelled nuts (18). Kernels are impacted onto steel plate and the resulting acoustic signal is analyzed to detect damage using different methods: modeling of the signal inthe time domain, computing time-domain signal variances and maximums in short-time win lows, analysis of the frequency spectrum magnitudes, and analysis of a derivative spectrum. Features used as inputs to a stepwise discriminant analysis, routine, which selected a small subset of features for accurate classification using a neural network, Pearson et al. (18) reported that impact: is a feasible and promising method for detection of IDK, sprout damage, and scab damage. More study is needed to improve accuracy on Kernels infested with insects that have not yet emerged from the ker nels. The computational cost of classify using this technique is very low, allowing inspection numbers of wheat kernels very rapidly, ~40 in inspectors usually use a 100g kernel) sample to inspect for IDK. This takes an inspec tor approximately 20 min to analyze manually, but can be accomplished in about 75 with an acou acoustic emissions ng a kernel of lary kernels/s. C «system, 19.5.6 Microscopy Techniques Microscopy techniques including light micro fluorescence microscopy, and scanning. electron microscopy (SEM) are used to study the struc ture/function relationships of food, but also can be applied to questions of extraneous matter. For exam ple, SEM with energy dispersive spectroscopy (EDS)pte 19. + Analysis or Extranoous Mater 364 can be used to determine the nature of metals in products that may be due to equipment failure or intentional adulteration due to tampering (19). Ligh! microscopy in a polarized mode can be used to dis tinguish between plastics, glass, and other fiber or rw contaminants (20) 19.5.7 Near-Infrared Spectroscopy Near-infrared spectroscopy (NIRS) isa relatively fast accurate, and economical technique available to the ain industry for compositional analysis such as ater, oll, fiber, starch, and protein in grains and seeds, It also has relativ applications in analysis of extraneous matter. NIRS has been used to identify several coleopteran species (21), sitized weevils in wheat kernels (2: internal insect infestation in wheat (23-25). Berardo et al. (26) reported that NIRS predicts the percentage of Fu ion in maize kernels and the content of ergosterol and fumosin BI in meals. Im the same way, promising results were obtained when NIRS methodology was applied to detect scab: damaged kernels (27) and estimate deoxynivalenol, exgosterol, and fumonisin in single kernels of wheat (21) and corn (28), Near-infrared spectroscopy used with a single ker- nel characterization system is able to detest later stages of internal insect infestation in wheat with a 95% conti: dence rocedures, this system is capable of being, automated and incorporated into the current grain inspection process. NIRS also has been compared with the current standard insect frag- ment flotation method for its ability to detect insect fragments in flour ( th both techniques were correlated; however, the flotation thod was more sensitive below the FDA DAL of insect fragments/S0g of wheat flour. NIR spec- troscopy was able to predict accurately whether flour samples contained less than or more than 130 frag: ments/50 , and to detect para and external and ticles inte 5). In contrast to other 9). Fragment counts 49.5.8 Enzyme-Linked Immunosorbent Assays To develop an optimal immunological assay for an insect contamination of foodstuffs, antibodies are required that are directed against an insect-specitic antigen, preferably protein, likely to be present in any life stage of the contaminating insect or in insect remains. Antigens and antibodie any immunoassay (see also Chap. 17 For an immunoassay with broad specificity it is required to us as myosin. are two key parts of an insect-specific protein such Myosin is ubiquitous in insects; it ts >resent in large quantities in adult insect tissue and Js also present in appreciable quantities in other life stages (30). An enzyme-linked immunosorbent assay (ELISA) method has been developed to measure quan- titatively the amount of insect material in a sample (30). It is also possible to develop an immunoassay specific for a particular species of insect contamination having a unique species specificity Kitto et al. (31) developed such techniques (patented in 1992) for detecting the amount of insect contamina- tion in foodstufls. The method comprises the follow ing steps: using antibod! 1, Preparing an aqueous solution or suspension of a homogenized grain sample Substantially affixing at least a portion of solu- ispension to a solid surtace to solid surface a specifically bind set antigen (or antibody) and enzyme to form an antibody-enzyme conjugate, result- ing in formation of a colored product when the enzyme reacts with a substrate 4. Washing unbound conjugate from the solid sur: face 5. Incubating the solid surface with an enayme substrate under conditions allowing colored ‘oduct to be formed when enzyme is present 6. Correlating amounts of color formed with an amount of insect contamina: tion ors Recent reseasch (32) showed that the myosin in fourth instars of the lesser grain borer developing within ker- nels of wheat degraded within the first 2 weeks when larvae were killed with phosphine, a famigant com. monly used to manage insect infestations in stored grain, Myosin degradation resulted in underestimat- ing insect fragment estimates by about 58' 19.6 COMPARISON OF METHODS A number of methods that have been developed to sects in com nodity samples (Table 19-3) are neral terms 1. Density separation based on infested kernels being lighter weight and floating in a liquid 2. Staining kernels to detect weevil egg plugs 3, Detection of carbon dioxide or uric acid pro- duced by the internally feeding insects 4. Detection of insects hiciien inside kemels usin, near-infrared spectroscopy (NIRS) 5, Detection by use of nuclear magnetic resonance (mR) 6. Detection by X-ray images and digital image analysis techniques362 Ltabie | insect Detection Methods Applicable for Commodity Samples (Adapied ftom (35) Test i w Applicability val inspection Sampling and sieving Heat extraction Acoustics Wrote grains Whole grains Breeding ou Imaging tectiniqu Xray method Whole grains Whole grains Near intrarea spectroscopy Nuclear magnetic resonance Serological techniques Urie acid determination 0, analysis Whole grains Spectic gravity methods, Whole grains Cracking and floatation ethos Fragment coun Whole grains Staining techniques Egg plugs Whole grains Ninhygirin method woke grains Acoustical sensors to hear sounds from insects feeding insicie kernels Enzyme-linked immunosorbent assays (ELISA) to detect myosin in insect muscle Some of the recent methods have been by adapting the single-kernel characterization sy: (SKCS), computed tomography (CT). ac fons, and use of a electrical conductive roller mill 3,34). The choice of method depends on several factors: a) type of infestation (inside or outs leveloped as, ide food grains, a Whole grains, milled produc Whole grains, milled produets Whole grains, milled products Whole grains, milled products Whole grains, milled products Whole grains, miled proaucts Ganments tative, only high-level infestation detected infestation not detectea Adults and larvae detected Feeding sounds: Active stages detected npact-acoustic emissions: Nondestructive, realtime; detect insect, sprout, ana scab damage Teme consuming Non-destructive, highly accurate, e to detect both live and dead secs inside grain kernels, cannot detect insect prohibitive capita co Rapid, sensitive, can be automated, ‘10 Sample preparation; cannot detect iow levels of infestation, senstive to moisture content, Calibration of equipment is, ccamprex and frequent Less sensitive sensitive, species spectic, restation from unknown past to til date ‘Shows infestation from unknown past to til date ‘Simple, ime consuming; indicates Current level of infestation; not suitable for grains having 15% moisture Simple and quick, not suitable for ats and maize Variable results noted ighiy variable results noted; shows infestation fromn unknown past to tidate pectic for Sitophius sop, Eggs and early larvae not indicated in the surrounding. premises or inside bulk grain) (b) required level af inspection (macroscopic vs. micro” scopic, qualitative vs. quantitative), (c) availability of equipment and facilitis,, and (d) required sensitivity (35). Most of the methods aim to detect the presence of live insects directly or indirectly. External insects are dete npling, sieving and heatextraction methods, while internal (hieden) insects are detected by radiography, staining tech niques to identify egg plugs, and near-infrared and Fragment count methods. Determination of uric acid or CO) level serves asan indirect way of detecting and by visual inspection, sanchapter 19. # Analysis or Exranaoue Mater 363 estimating internally feeding insects, and these meth: ods may be suitable if infestations are restricted to one insect species. Depending on some storage conditions, grain may contain molds and insects, and in such cases CO, produced by molds may interfere in accu rately detecting or estimatin and ELISA methods can be used for the detection of both living and dead insects. In general, problems encountered with these detection methods are that the most accurate methods, such as X-ray and computed tomography (CT), are laborious and expensive, while rapid, automated methods may not be suitable for detecting eggs and young larvae (32) insects. Fragment count 19.7 ISOLATION PRINCIPLES APPLIED TO FOOD PROCESSING Examination of stored-product insects often requires extracting them from the commodity. An intensive summary of literature survey on insect extraction and detection methods can be found in reference (36). Iso- lation principles, such as particle size and density, discussed in the preceding sections are designed to identify extraneous materials in finished food prod uucts, monitoring quality, and compliance with DALs. In addition, some of these principles of isolation are used in a proactive way during processing to pre- vent extraneous matter from being incorporated into finished food products. ‘Wheat that contains hidden internal insect infes tation is the primary source of insect fragments in processed cereal products, The current DAL for inter al insect infestation in wheat is 32 IDK per 100g of wheat (3). IDK are those visually determined to have insect tunneling or emergence holes. Most processors rely on much lower levels of IDK (<6 IDK/100g) to produce flour that meets customer tolerances and the FDA’s DAL tor insect fragments in flour. In addition, to prevent adulteration of flour with filth, entoleters royers in the milling process break id kerncls, and these broken kernels sect fragments are aspirated out of the X-ray radiog- electing grains for processing or for research purposes 10 age-grade internally developing, rain insects More recently, NIR spectroscopy has provided a new tool for assessing internal insect infestation in whea By selectively milling only wheat that has minimal or no evivience of internal insect infestation, grain pro- cessors can effectively limit insect fragments in their products. In like manner, bakers and other users of processed grain products can selectively monitor for sect fragments in their raw materials using one of and infestation de up insect-damaj along with the i milling stream. As previously indicate raphy is used by some as a means f the approved methods for extraction and enuintera~ tion of fragments or by sendi samples to a private laboratory for fragment analysis. Most food processing systems that deal with agri cultural products generally apply some type of clean. ing operations as an initial step. In flour milling, for example, wheat is passed through a system called the “cleaning house,” which consists of a series of ‘machines that apply the principles of particle size and density separation. Sieves remove contaminants larget than wheat kernels as well as finer contaminants s as sand. In addition, ait (aspiration) is used to remove plant material that is lighter than the grain. Current equipment to remove stones and other dense materials the same size as grain kernels use air passed upward through an inclined, tilted table. This causes the grain to “float” off the side of the table and the heavier mate- rial fo continue and “tail” over the end of the table In earlier systems, grains were passed through wash- ecs in which water separated th material (such as stones) much like fluming of pota- toes or fruit does. Impact with rotating disks and steel pegs (entoleters and infestation destroyers) or grind ing operations are used prior to milling to break open kernels of wheat containing intemal insect infestation As a means of reducing insect fragments in the fin ished product, this process is followed by aspiration to lift out any light insect contaminants released in the operation As a final step in wheat milling, flour is gen erally passed through sieves fine enough to remove insect eggs and any other contaminants that might be present, This is to assure that when flour leaves the mill it is free of any viable form: of insect contamina- ton (37). Where flour is used in large quantities, such as commercial bakeries, prior to use, flour is again sieved to ensure that no contamination has occurred ansport and storage of the flour Metal contamination has been a major concern of all food processors, Although metal detection meth- ods are not specifically among the isolation techniques represented in AOAC International or ACC Inter national methods manuals, they serve the purpose of isolating contaminants from food products, Magnets of various types have been used on raw materials and processing systems to prevent the passage of metal into handling and processing equipment where both equipment damage and product contamination arc concerns, Metal detectors are employed in many food processing operations and on finished product pack: aging lines to detect ferrous and nonferrous metal fragments and to prevent contaminated products from entering consumer food channels. Recent X-ray technology suggests that X rays may have an advantage over other methods for detecting metal and that they can also be used to detect glass, grain from heavier364 Parti! * Chemical Pronertes and Characters wood, plastic, and bon chips in foods. Detection of 19.10 ACKNOWLEDGEMENT these extraneous materials also can be automated with ng lines (38). This contribution is paper number 10-062-B of the rejection systems in packagi Kansas Agricultural Experiment Station, Kansas State University, Manhattan, KS 66506. 19.8 SUMMARY Extraneous matter in raw ingredients and in processe 19.11 REFERENCES: foods might be unavoidable in the array of foods that are stored, handled, processed, and transported, DALs 1. FDLI (1993) Federal food drug and cosmetic ac are established for amounts considered unavoidable amended. In: Compilation of food and drug laws. The and of no health hazard, A variety of methods are Food and Drug Law Institute, Washington, DC availiole 0 isolate extraneous matter from foods. 2 FDA (2009) Cucrent Those methods largely prescribed by AOAC manufacturing, packin sane non a cetet ob ahwcicahanclchesucal wenn 110, Title 21: food and deugs, In: Code of federal regu tional employ a series of physical and chemical means ations. Office of the Federal Register National Archives and Records Administration, Washington, DC jon. Major concerns in the analysis of 3, FDA {1905} The lend west mc for extraneous matter are the objectivi od manufacturing practice in ‘of holding human food. Pa terna to separate the extraneous material for identification food produc ect action levels ~ custent lev ral or unavoidable defects for human use of methods and the availability of adequately trained that present no health hazard (revised 1998), Depart analysts. Some “p-inciples” of isolation are applied ia ment of Health and Human Services, Food and Drug a proactive way in food processing operations. Administration, Washington, DC Currently available methods (both macroscopic 4. FDA (2000) Compliance policy guide manual. Food and microscopic) show varying degrees of efficiency and Drug Administration, Office of Regulatory Af n analysis of extraneous maiter and filth in foods Washington, DC ee AOAC international (2007) Extraneous materials: isle personnel, and are difficult to implement in real time tion. In: Horwitz W, Latimer G (eds) Official methods ome techniques are time-consumin ‘of analysis, 18th edn, 2005; Custent through evision 2, 204? (on-line). 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Food Science 745 Agriculture Mall Di West Lafayette IN 479 USA nielse: mpurdueedu eISBN 978-1-4419-1478:1 ISBN 978.4-4119-147 DO} 10,1007/978-1-4419-1478-1 pringet Now York Dordrecht Heidelberg Londor ary of Congress Control Number: 2020924120 Springer Scence+Busintss Media, LLC 2010 fi be tanslated or copied in whole ot in part without the writen permission ofthe publisher (Springer Science: Busines 33 Spring Stree, Uow York, NY 10013, USA} except for brie! excerpts in connection with reviews or cho lav analysis, se in connection with ary form of informatien storage and retrieval, electronic adaptation, computer software, or by similac (oF dissimilar methodology now known ot hereafter developed is forbid The uae inthis publication of trade names, trademarks, servicemarks, nd silax terms even if they are not identified as such isnot to be taken as an expression of opinion as 0 whether or nc hey are subject to propeletary High Printed on acic-tee pape Springeris partof Springer Science+Business Medi (www springercom)