ExFHPB-1 Determination of Extraneous Material in Alimentary Paste Products

1、ExFHPB-1 Determination of Extraneous Material in Alimentary Paste Products Government of Canada Gouvernement du Canada HPB MethodExFHPB-1March 2009HEALTH PRODUCTS AND FOOD BRANCHOTTAWADETERMINATION OF EXTRANEOUS MATERIAL IN ALIMENTARY PASTE PRODUCTSEva PietrzakNational Manager, Food Microbiology and

2、 Extraneous Matter Evaluation Section,Food Safety Division, CFIAthTower 2, 94 floor, Rm 153,1440 MerivaleOttawa, ON.K1A 0Y98E-mail: Eva.Pietrzakinspection.gc.ca1.APPLICATIONThis method is applicable to the enumeration of extraneous material light filth elements, such as insects, insectfragments, mit

3、es, hairs, and feather barbules, and heavy filth particles, such as sand, soil, metal, glass, insectand rodent excreta pellets, in alimentary paste products to determine compliance with Sections 4, 5 and 7 ofthe Food and Drugs Act. This method replaces ExFHPB-1 dated January 2006. 2.DEFINITION OF TE

4、RMSA lot is defined as that amount (volume, weight, etc.) of the food which is produced, stored and/or shippedunder conditions as nearly uniform as possible, preferably designated by a common container code or markingand in any event, consisting of not more than one variety, grade or type of product

5、 from a single identifiablesource.3.COLLECTION OF SAMPLES3.1Scrutinize the entire lot for live infestation. If live infestation is found, do not sample until afterfumigation or other effective treatment.3.2Obtain three sample units selected at random from the lot of at least 225 g each using appropr

6、iatesampling equipment and containers. Three sample units constitute a sample.3.3Each sample unit must be kept separate and labelled 1, 2, 3. Complete information respecting thelot size, weight of individual containers, country of origin, exporter, importer or domestic manufacturerand product and lo

7、t identification should be recorded and should accompany the sample.4.MATERIALS AND SPECIAL EQUIPMENT1)Balance2)2 - 2.0 L beakers and lids (watch glasses)Published on the Food Directorates (Health Canadas) website at /.hc-sc.gc.ca/fn-an/res-rech/analy-meth/microbio/index_e.phpExFHPB-01- 2 -March 200

8、93)Autoclave. Either (a) slow exhaust type (Set slow exhaust to lower pressure from 1.15 to 0 kg per sq.cm in 15-20 min.) or (b) non-slow exhaust (Let cool to 0 kg per sq. cm before opening or venting)4)U.S. standard No. 230 sieve5)Shallow pan $ 20 cm in diameter6)Smooth magnetic stirring bar, teflo

9、n coated (1 x 5 cm)7)Stirrer hot plate8)2 L percolator, premarked at 250 and 1700 mL levels9)Wash bottles10)Rubber policeman11)Suction filtration apparatus with Buchner or Hirsch funnel (5-7 cm perforated plate)12)Ruled filter paper. Filter paper should be larger than funnel plate (7-9 cm)13)Petri d

10、ishes to suit size of filter paper used14)Stereoscopic microscope (10-30x)15)Ashless filter paper. Filter paper should be larger than funnel plate (7-9 cm)o16)Drying oven (40-60C)17)Crucible18)Desiccator19)Muffle oven20)Concentrated HCl21)Antifoam solution. BDH Antifoam B22)Detergent, 1% sodium laur

11、yl sulphateo23)Mineral oil. Paraffin oil, white, light 125/135 Saybolt Universal Viscosity (38C), specific gravity 0.840-o0.860 (24C)24)Alcohol, either 95% ethanol or 99% isopropanol25)Glycerol-alcohol (95%) mixture (1:1)26)Chloroform (CHCl)35.PROCEDUREThe examination shall be carried out in accorda

12、nce with the following instructions.5.1Preparation of Analytical Units5.1.1Thoroughly mix a sample unit and weigh 225 g of alimentary paste. This 225 g constitutes ananalytical unit.ExFHPB-01- 3 -March 20095.1.2Repeat step 5.1.1 for remaining two sample units.5.2Isolation - Light Filth5.2.1Transfer

13、an analytical unit to a 2 L beaker. For spaghetti, break into lengths that will not lieflat on bottom of beaker. If large amounts of spaghetti lie on the bottom they may not digestcompletely.5.2.2Add 1 L HCl (30 mL concentrated HCl + 970 mL water), 0.3 mL of antifoam solution andcover with a lid. Se

14、t beaker in a larger container in case of breakage.o5.2.3Autoclave for 30 min. at 121C. Caution: check autoclave periodically for corrosive damage.o5.2.4Wet sieve on a No. 230 sieve with hot tap water (50-70C) to remove all original liquid anda major portion of fine material.5.2.5If there is any fat

15、 material remaining defat as follows. Place sieve in a shallow pan, coveroresidue to a depth of approximately 2 cm with hot (50-70C) detergent, leave for 5 min., drainand wet sieve with hot tap water until all suds have washed through. Be careful not to allowsuds to foam over sides of sieve. Repeat

16、defatting procedure at least once or until all visiblefat has been removed.o5.2.6Transfer sieve retainings to original beaker with hot water (50-70C) and dilute toapproximately 1 L. Add 30 mL conc. HCl, a magnetic stirring bar and 50 mL of mineral oil.5.2.7Stir magnetically at maximum speed that doe

17、s not produce visible or audible splashing for6 min.5.2.8Promptly transfer contents of beaker to a percolator containing approximately 250 mL ofwater. Rinse contents of beaker into percolator with hot tap water making certain to transferall material including heavy filth. Bring volume in percolator

18、to 1700 mL with hot tap water.5.2.9Using wash bottles, rinse magnetic particles from stirring bar into a beaker first with water,then alcohol and finally with detergent until all particles are washed off. Filter washingsthrough ruled filter paper using suction filtration apparatus. Transfer filter p

19、aper to a petri dishand moisten with glycerol-alcohol mixture.5.2.10After 3 min., drain oil interface in percolator to 250 mL into a 2 L beaker. Retain contents ofbeaker for heavy filth determination.5.2.11Refill percolator by pouring hot tap water down percolator sides to loosen adhering materialan

20、d refill to 1700 mL mark.5.2.12After 2-3 min., drain percolator to 250 mL, discard drainings and refill for 2 more cycles.Lower layer should be almost free of suspended material after refill. If not continue through$ 1 recycles.5.2.13Finally, drain oil-water interface to 250 mL mark and drain remain

21、ing contents into originalbeaker. Promptly, using wash bottles, wash down sides of percolator successively with $ 50mL portions of hot tap water, alcohol and hot tap water. Use detergent if necessary.5.2.14Using suction filtration apparatus, filter beaker contents through ruled filter paper with ami

22、nimum of 50 mL washes of hot water, alcohol and water or detergent. Use a rubberpoliceman if necessary to clean sides of beaker.5.2.15Transfer filter paper(s) to petri dish(es) and moisten with glycerol-alcohol mixture.ExFHPB-01- 4 -March 20095.3Examination - Light FilthExamine paper(s) microscopica

23、lly at 30X magnification for all types of extraneous material. Use ahigher magnification (70X) only to confirm questionable particles.5.4Recording Results - Light Filth5.4.1Classify insect fragments into the following three categories:a)Premilling insect fragments ( # 0.595 mm) that can not be ident

24、ified or are identifiedas field insects (see Tables 1 and 2);b)Premilling insect fragments ( # 0.595 mm) that are identified as stored food insects(see Tables 2 and 3);c)Postmilling insect fragments ( > 0.595 mm) that can not be identified or are identifiedas stored food insects (see Tables 2 and

25、 3).5.4.2Record the number and range in size (mm) of all light filth elements separately for eachanalytical unit.5.5Isolation - Heavy Filth5.5.1Stir contents of beaker containing drainings from Light Filth, Step 5.2.10, with rubberpoliceman for 30 sec. and allow suspension to stand undisturbed for 3

26、0 min.5.5.2Decant suspended food material without disturbing bottom contents.5.5.3Add 400-500 mL of water, stir 30 sec. and let stand 10 min.5.5.4Repeat steps 2-3 until practically all plant tissue has been decanted.5.5.5If any heavy filth is present, add 100-200 mL of CHCl, stir 30 sec., let stand

27、10 min. and then3decant water layer (top layer) without disturbing or pouring off any of CHCl-water interface.35.5.6Filter contents of beaker onto an oven-dried preweighed ashless paper. Transfer filter paperto petri dish.5.6Examination - Heavy FilthExamine filter paper microscopically at 30x magnif

28、ication for rodent pellets, insect excreta, insectlarvae, insect eggs and other organic filth.5.7Recording Results - Heavy Filth5.7.1Record the number and range in size of each type of heavy filth detected for each analyticalunit separately.5.7.2Dry filter paper in an oven and weigh. Determine weigh

29、t of heavy filth by difference.5.7.3If there is an appreciable amount of residue, transfer filter paper with contents to aopreweighed crucible and ash in a muffle oven at approximately 500C for two hr. Coolmaterial in a desiccator and weigh. Determine ashed weight by difference and record.ExFHPB-01-

30、 5 -March 20096.INTERPRETATION6.1See Table 1 of ;Guidelines for the General Cleanliness of Food - An Overview; found in Volume I ofthe Compendium of Analytical Methods for guidelines relating to different types of extraneousmaterials in alimentary paste, semolina derived only.6.2If there is a questi

31、on as to the acceptability of the lot, contact:Eva PietrzakNational Manager, Food Microbiology and Extraneous Matter Evaluation Section,Food Safety Division, CFIAthTower 2, 4 floor, Rm 153,1440 MerivaleOttawa, ON.K1A 0Y9E-mail: Eva.Pietrzakinspection.gc.caPhone: 613-773-5812 FAX: 613-773-5957Table 1

32、. Examples of field insectsCommon NameOrderarmywormsLepidopterasawfliesHymenopterajointwormsHymenopterastrawwormsHymenopteragrasshoppersOrthopteraaphidsHomopterabugsHemipterahessian fliesDipteramidgesDipterathripsThysanopteraExFHPB-01- 6 -March 2009Table 2. Examples of insects infesting whole undama

33、ged grains in storage. These insects may also attack grains inthe field in warm climates.SpeciesFamilyCommon NameORDER: ColeopteraRhyzopertha dominica (Fabricius)Bostrichidaelesser grain borerSitophilus granarius (L.)Curculionidaegranary weevilSitophilus oryzae (L.)Curculionidaerice weevilSitophilus

34、 zeamais (Motschulsky)Curculionidaemaize weevilORDER: LepidopteraSitotroga cerealella (Olivier)GelechiidaeAngoumois grain mothExFHPB-01- 7 -March 2009Table 3. Common insects infesting damaged and milled grain SpeciesFamilyCommon NameORDER: ColeopteraAlphitobius diaperinus (Panzer)Tenebrionidaelesser mealwormCryptolestes capensis (Waltl)Cucujidaecape grain beetleCryptolestes ferrugineusCucujidaerusty grain beetle(Stephens)Cryptolestes pusillus (Sch?nherr