ASTM E1396-90(2017) Standard Test Method for Sensory Evaluation of Oleoresin Capsicum.pdf

1、Designation: E1396 90 (Reapproved 2017)Standard Test Method forSensory Evaluation of Oleoresin Capsicum1This standard is issued under the fixed designation E1396; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last rev

2、ision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method describes standardized procedures forthe sensory evaluation of heat in oleoresin capsicums rangingfrom 100 00

3、0 to 1 000 000 Scoville heat units (S.H.U.).1.2 This test method is intended as an alternative to theScoville heat test, but results can be expressed in Scoville heatunits (see ASTA Method 21.0 and ISO 3513).1.3 This test method does not apply for ground red pepper,low heat chili peppers, or chili p

4、owder.1.4 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.5 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establis

5、h appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. Specific precau-tionary statements are given in Section 8.2. Referenced Documents2.1 ASTM Standards:E1083 Test Method for Sensory Evaluation of Red PepperHeat22.2 ASTA Standard:ASTA Me

6、thod 21.0 Official Analytical Methods32.3 ISO Standard:ISO 3513-1977 (E), Spices and Condiments-Chilies-Determination of Scoville Index42.4 AOAC Method:Official Methods ofAssociation of OfficialAnalytical Chem-ists International (1996) 995.03 (43.1.43)3. Terminology3.1 Definitions of Terms Specific

7、to This Standard:3.1.1 approaching strong heatN-vanillyl-n-nonamide,1.30 ppm. This is 13.0 cm on the 15-cm line scale. It is unusualto see an oleoresin stronger than this. But in the event that apepper with more than expected heat is tested, there remainsthe last 2 cm on the 15-cm line scale.3.1.2 m

8、oderate heatN-vanillyl-n-nonamide, 0.80 ppm.This is a “moderate” amount of pepper heat. It reads 10 cm onthe 15-cm line scale.3.1.3 rinseto purge the oral cavity with unsalted sodacrackers and 20C spring or distilled water by slowly chewingand swallowing the cracker, followed by swirling the waterar

9、ound in the mouth and swallowing. This procedure isrepeated as often as is natural and comfortable for the panelist.3.1.4 Scoville heat units (S.H.U.)the commonly acceptedunit for expressing heat levels in capsicum products (see TestMethod E1083 and ASTA Method 21.0). Scoville heat unitsrange from 0

10、 to 1 500 000.3.1.5 slight heatN-vanillyl-n-nonamide, 0.40 ppm. This isa “slight” amount of pepper heat. It reads 5 cm on the 15-cmline scale.3.1.6 strong heatbest defined by concept. Hotter than the1.30-ppm N-vanillyl-n-nonamide sample. It reads 15 cm on the15-cm line scale.3.1.7 threshold heatbest

11、 defined by concept rather than bya standard dilution of N-vanillyl-n-nonamide. Threshold is thatpoint where a panelist just barely senses burn/heat. It reads1.25 cm on the 15-cm line scale.3.1.8 zero heatN-vanillyl-n-nonamide, 0 ppm. No sensoryheat. It reads 0 cm on the line scale.4. Summary of Tes

12、t Method4.1 Oleoresin capsicum is steeped in hot water withpolysorbate-80 or polysorbate-60 for 3 min, filtered, and thefiltrate diluted in room temperature water. Trained panelists1This test method is under the jurisdiction of ASTM Committee E18 on SensoryEvaluation and is the direct responsibility

13、 of Subcommittee E18.06 on Food andBeverage Evaluation.Current edition approved Feb. 1, 2017. Published February 2017. Originallyapproved in 1990. Last previous edition approved in 2011 as E1396 90 (2011).DOI: 10.1520/E1396-90R17.2For referenced ASTM standards, visit the ASTM website, www.astm.org,

14、orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Available from American Spice Trade Association, Box 1267, EnglewoodCliffs, NJ 07632.4Available from American National Standards I

15、nstitute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036, http:/www.ansi.org.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on sta

16、ndardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.1compare the heat in the pepper extract to a known concentra-tion of a standard solution

17、 of synthetic capsaicin (N-vanillyl-n-nonamide) using a 15-cm line scale. The tasting procedure istimed and takes 2 min for one test sample and 9 min for twotest samples.5This test method is a minor variation on theground red pepper sensory method.4.2 Panelists are screened for their accuracy and pr

18、ecisionand trained to use the 15-cm line scale during two to three15-min training sessions.4.3 Standard general requirements for sensory testing fol-lows.45. Significance and Use5.1 This test method provides quick and accurate ratings forthe sensory heat in oleoresin capsicums ranging from 100 000to

19、 1 000 000 Scoville heat units.5.2 Sensory results from this test method correlate highly(r2= 0.94) with results from high pressure liquid chromatog-raphy; making the two methods substitutable.66. Apparatus6.1 Magnetic Hot Plate Stirrers, two.6.2 Beakers, 600-mL, four.6.3 Small Beaker, 50 to 100 mL.

20、6.4 Analytical Balance, capacity greater than 300 g, sensi-tive to 0.01 g.6.5 Volumetric Flasks, 1000-mL stoppered, two.6.6 Stopwatch.7. Reagents and Materials7.1 Coffee Filter Papers, or low flavor qualitative filterpaper.7.2 Medicine Cups.7.3 Unsalted Soda Crackers, unsalted tops.7.4 Water, bottle

21、d, distilled, or deionized when available, orstill spring water.7.5 Polysorbate-80 or Polysorbate-60, food grade.7.6 Rating Forms, 15-cm line scale anchored at 0 (none),1.25 cm (threshold), 5 cm (slight), 10 cm (moderate), 15 cm(strong); see Appendix X1.7.7 N-vanillyl-n-nonamide, available from Pent

22、a Interna-tional (some restrictions apply).8. Precautions8.1 Pure N-vanillyl-n-nonamide will burn the eyes and skinupon direct contact. Gloves and caution must be used whenhandling N-vanillyl-n-nonamide in the crystalline form.9. Calibration and Standardization of Panelists9.1 Select ten to twelve p

23、anelists based on availability,attitude, and motivation of panelists. Screening for tastesensitivity is not necessary.9.2 Prepare stock solution of N-vanillyl-n-nonamide (see10.1.2).9.3 Dilute the stock solution of N-vanillyl-n-nonamide tothe following concentrations:9.3.1 N-vanillyl-n-nonamide, 0 p

24、pmAdd none of the stocksolution to 200 mL of water.9.3.2 N-vanillyl-n-nonamide, 0.40 ppmDilute 13.4 g ofstock solution to 200 mL with water.9.3.3 N-vanillyl-n-nonamide, 0.80 ppmDilute 26.8 g ofthe stock solution to 200 mL with water.9.3.4 N-vanillyl-n-nonamide, 1.30 ppmDilute 43.3 g ofthe stock solu

25、tion to 200 mL with water.9.4 Session 1 (15 min)Brief the panelists on the purposeof this test method. The purpose of the first session is tostandardize their tongues and mouth to the reference standardswith respect to the 15-cm line scale on the ballot (see Fig. 1).Explain to the panelists that the

26、y may use any of the infinitenumber of points on the line scale to describe how hot a givensample is. Panelists will taste (see 10.2.3.1 10.2.3.3) thecoded standard dilutions prepared, evaluate them critically,concentrating and memorizing their individual sensory heatlevels. Panelists rinse well bet

27、ween samples with unsalted sodacrackers and spring or distilled water for 2 min (they aretimed). After the standards have been tasted, the correct ratingfor each reference standard is given. A new set of labeledstandard dilutions is presented to the panelists to review.Definitions for “0,” “threshol

28、d,” “slight,” “moderate,” “ap-proaching strong,” and “strong” are provided. Refer to 3.1.1,3.1.2, 3.1.6, 3.1.7, and 3.1.8.9.5 Session 2 (15 min)This session should follow the firsttraining session by one to two days. During this session, thepanelists will be both trained and tested. Explain to thepa

29、nelists how they will be evaluating the actual red pepper testsamples. Explain the entire tasting procedure as follows:5Gillette, M. H., Appel, C. E., and Lego, M., “A New Method for the SensoryEvaluation of Red Pepper Heat,” Journal of Food and Science, Vol 49, No. 4, 1984,p. 1028.6Hoffman, P. G.,

30、Salb, M. C., and Galetto, W. G., “Separation and Quantitationof Red Pepper Heat Principles by Reverse Phase HPLC,” Journal of Agriculturaland Food Chemistry, Vol 31, No. 6, Oct. 1983, p. 1326. FIG. 1 Oleoresin Capsicum Heat Sensory versus HPLCE1396 90 (2017)29.5.1 Panelists are served 10-mL portions

31、 of each of twosamples in coded medicine cups. The control (0.4-ppmN-vanillyl-n-nonamide) is always served first, coded “C.” Thetest sample is served second, with a random two-letter code.Two sets of samples are evaluated per sitting. The tastingprocedure is described in 10.2.3.9.5.2 For this second

32、 training session, the panelists areserved the “control” first, coded “C,” then a test sample codedwith a random two letter code. They will evaluate two sets ofsamples:9.5.2.1 Control and 0.80 ppm N-vanillyl-n-nonamide.9.5.2.2 Control and 0.40 ppm N-vanillyl-n-nonamide (thesame as the control).9.5.2

33、.3 Do not tell the panelists what the test samples are.After learning the standard heat intensities during Session 1,they theoretically should rate the 0.80-ppm sample at “moder-ate” and the 0.40-ppm sample at “slight” on the line scale. A2-cm variation from the desired response is acceptable. Thepa

34、nel, as a whole, should also be within 2 cm of the desiredresponse. If not, another training session must be conducted.After the session, advise the panelists about the sampleidentities and the expected ratings for them. Panelists mustreproduce their judgment within 2 cm of the desired response.A mi

35、nimum of five panelists should pass for the formal testing.Repeat training until this is achieved (approximately threetraining sessions).9.5.2.4 End the training session by giving the panelists asample of oleoresin capsicum to acquaint panelists with theflavor of chili peppers (not present in the st

36、andards).10. Procedure10.1 Sample Preparation:10.1.1 Sample preparation procedures are itemized in aquick reference chart (see Appendix X1).10.1.2 Evaluate two samples per test: (1) a known control(0.40 ppm dilution of N-vanillyl-n-nonamide) prepared fromthe stock solution; and (2) the unknown oleor

37、esin capsicum.Preparation of the two samples is as follows:10.1.3 Prepare the “stock” solution of N-vanillyl-n-nonamide (6 ppm N-vanillyl-n-nonamide and 200 ppmpolysorbate-80 or polysorbate-60) by diluting N-vanillyl-n-nonamide and polysorbate-80 or polysorbate-60 in spring ordistilled water. Keep t

38、his solution stoppered and refrigeratedfor the duration of the test series. It will remain stable for 2 to3 weeks. Check regularly for precipitation of N-vanillyl-n-nonamide. To make the stock solution, weigh 0.60 gN-vanillyl-n-nonamide and 20 g of polysorbate-80 orpolysorbate-60 into a small beaker

39、 (50 mL). Heat the mixtureon a hot plate (low setting) for a minimum of 10 min todissolve N-vanillyl-n-nonamide. Quantitatively transfer theheated mixture into a 1-L volumetric flask using hot (about70C) spring or distilled water. Cool to room temperature.Dilute the transferred solution to 1 L using

40、 room temperature(20C) spring or distilled water. Dilute 10 g of this solution to1 L in a second 1-L volumetric flask. Stopper and refrigerate.Final concentrations equal 6 ppm N-vanillyl-n-nonamide, 200ppm polysorbate-80 or polysorbate-60. This is a “stock solu-tion.”10.1.4 For each test, dilute the

41、 stock solution of N-vanillyl-n-nonamide to 0.40 ppm N-vanillyl-n-nonamide and 13.3 ppmpolysorbate-80 or polysorbate-60 in 20C spring or distilledwater by diluting 13.4 g of the stock solution to 200 mL withroom temperature water. This diluted solution is referred to asthe “control” for each test.10

42、.1.5 Oleoresin Capsicum SamplesOn the day of the test,add 0.1 g of the oleoresin sample directly to 0.2 g ofpolysorbate-80 or polysorbate-60 and heated at 200C for 1min in a 600-mL beaker, diluted to 400 mL with 70C springor distilled water and place on the preheated (medium heat;200C) hot plate sti

43、rrer on medium stir speed for 2 min. Dilute5 mL of the extract to 200 mL using 20C spring or distilledwater. Final concentration of the extracted and diluted solutionis 6.25 ppm oleoresin and 12.5 ppm polysorbate-80 orpolysorbate-60.10.2 Sample Presentation:10.2.1 A round or conference table is pref

44、erred, but boothsmay be used as long as all panelists are able to be “monitored”by the panel leader. Conduct the test with all five to ten trainedpanelists simultaneously as the process is timed by the panelleader (if a panelist misses a panel, he/she must also be timedduring his/her “make-up” test)

45、. Red lights are recommended tomask color differences.10.2.2 Serve panelists 10-mL portions of each sample incoded medicine cups. Serving temperature should be at roomtemperature and equal for all samples. The control is alwaysserved first, coded “C.” The test sample is served second, witha random t

46、wo-digit code. Evaluate two sets of samples (controland test sample) per sitting. Use a 15-cm line scale anchored at0 cm (0 heat), 1.25 cm (threshold heat), 5.0 cm (slight heat),10.0 cm (moderate heat), and 15 cm (strong heat) (see X1.2).Use a separate scale for each set of samples. Order ofpresenta

47、tion of the sample sets should be balanced to avoidposition bias.10.2.3 The testing procedure is as follows:10.2.3.1 Rinse before first sample (control) with unsaltedsoda cracker and 20C spring or distilled water, or both. Allow15 s between rinsing and sampling.10.2.3.2 Evaluating left to right, tak

48、e entire first sample(control) in mouth, hold for about 5 s, swallow slowly.10.2.3.3 Wait 30 s (timed) from initial intake keeping mouthclosed.10.2.3.4 Rate first sample at “slight” on ballot.10.2.3.5 Alternately rinse with 20C spring or distilledwater and chew on an unsalted soda cracker during a 6

49、0-sinterval (timed).10.2.3.6 Rinse with 20C spring water immediately prior tosecond sample. Allow 15 s between rinsing and sampling.10.2.3.7 Take entire second sample (test sample) in mouth,hold for about 5 s, swallow slowly.10.2.3.8 Wait 30 s (timed), keeping mouth closed.10.2.3.9 Rate second sample.10.2.3.10 Panel dismissed if only one test sample is to beevaluated.10.2.3.11 If two test samples are to be evaluated, wait 5 min(timed). Rinse well with spring or distilled water and unsaltedcrackers during this time.E1396 90 (2017)310.2.3.