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AOAC 996.06 Fat in Food鱼油的检测方法1

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AOAC 996.06 Fat in Food鱼油的检测方法1 搜索文档 在手机打开 0 下载券  下载

C. Re agents
41.1.28A 相关文
AOAC Official Method 996.06 (a) Pyrogallic acid.
Fat (Total, Saturated, and Unsaturated) (b) Hydrochloric acid.—12 and 8.3M. To make 8.3M HCl, add Bla
in Foods 250 mL 12M HCl to 110 mL H 2O. Mix well. Store at room ww
Hydrolytic Extraction Gas Chromatographic Method temperature (20°–25°C). A
First Action 1996 (c) Ammonium hydroxide.—58% (w/w).
Revised 2001
(d) Diethyl ether.—Purity appropriate for fat extraction.
(Applicable to determination of fat in foods.) A
(e) Petroleum ether.—Anhydrous.

Caution: Boron trifluoride may be fa tal if in haled. (f) Ethanol.—95% (v/v). 面

(g) Toluene.—Nanograde.
See Tables 996.06A–C for the results of the interlaboratory study (h) Chloroform.
supporting acceptance of the method. (i) Sodium sulfate.—Anhydrous. A
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A. Principle (j) Boron trifluoride reagent.—7% BF3 (w/w) in metha  nol, made
from commercially available 14% BF3 solution. Prepare in the hood. 鱼油的
Fat and fatty acids are extracted from food by hydrolytic meth ods
(acidic hydrolysis for most products, alkaline hydrolysis for dairy (k) Diethyl ether–petroleum ether mixture.—1 + 1 (v/v). 喜欢此
products, and com bination for cheese). Pyrogallic acid is added to (l) Triglyceride internal standard solution.—C11:0-triundecanoin;
A
minimize oxidative degradation of fatty acids during analysis. 5.00 mg/mL in CHCl3. Accurately weigh 2.50 g C11:0-triundecanoin
Triglyceride, triundecanoin (C 11:0), is added as internal standard. Fat into 500 mL volum  etric flask. Add ca 400 mL CHCl3 and mix until
is ex tracted into ether, then meth ylated to fatty acid methyl es ters dissolved. Di lute to vol ume with CHCl 3. In vert flask at least A
(FAMEs) using BF3 in metha  nol. FAMEs are quantitatively measured 10 additional times. Triglyceride internal standard solution is
by capillary gas chromatography (GC) against C11:0 internal standard. stable up to 1 month when stored in re frigera  tor (2°–8°C).
Total fat is cal culated as sum of in dividual fatty ac ids ex pressed as             
( m ) F a t t y a c i d m e t h y l e s t e r s ( FA M E s ) s t a n d a rd A
triglyceride equiv a  lents. Sat u 
rated and monounsaturated fats are solutions.—(1) Mixed FAMEs stan dard so lution.—Reference
calculated as sum of re spective fatty ac ids. Monounsaturated fat mixture containing series of FAMEs, including C18:1 cis and trans A
includes only cis form. (avail able
USA, as GLC-85
or equiv a  from
lent). To preNu Chek
pare Prep,
mixed Ely stan
FAMEs sian,dard
MNso56028,
lution,
B. Apparatus
break top of glass vial, open, and care fully trans fer con tents to A
(a) Gas chromatograph. —With hydrogen flame ionization 3-dram glass vial. Wash orig in al vial with hex ane to en sure
detector, capillary column, split mode injector, oven temperature  
complete transfer and add washings to 3-dram glass vial. Di lute to ca
programming sufficient to implement a hold-ramp-hold sequence. 3 mL with hex ane.
Operating conditions: temperature (°C): injector, 225; detector, 285; (2) C11:0 FAME standard solution.—C11:0-Undecanoic methyl
initial temp, 100 (hold 4 min); ramp, 3°C/min; final temp 240; hold ester in hex ane. Use only in prep a  ration of in dividual FAME
15 min; carrier gas, helium; flow rate, 0.75 mL/min; linear velocity, standard solutions, (3). To pre pare C 11:0 FAME stan dard so lution,
18 cm/s; split ra tio, 200:1. break top of glass vial open and carefully transfer contents to 50 mL
(b) Capillary column.—Sepa  rating the FAME pair of ad jacent volu  metric flask. Wash origi 
nal vial with hexane to ensure complete
peaks of C18:3 and C20:1 and the FAME trio of adjacent peaks of C22:1, transfer and add washings to 50 mL vol u  metric flask. Di lute to
C20:3, and C20:4 with a resol ution of 1.0 or greater. SP2560 100 m ´ volume with hex ane. C 11:0 FAME stan dard so lution is sta ble up to
0.25 mm with 0.20 mm film is suit able. 1 week when stored at 0°C.
(c) Mojonnier flasks. (3) Individual FAME standard solutions.—Standard solutions of
(d) Stoppers.—Synthetic rubber or cork. each of fol low ing FAMEs: C 4 : 0 -tetranoic methyl es ter,
(e) Mojonnier centrifuge basket. C 6 : 0 -hexanoic methyl es ter, C 8 : 0 -octanoic methyl es ter,

(f) 10:0 -decanoic methyl es ter, C 12:0 -dodecanoic methyl es ter,

(g) Hengar mi cro boil
Baskets.—Alu minuming gran ules.tic.
and plas C
C13:0-tridecanoic methyl es ter, C 14:0-tetradecanoic methyl es ter,
(h) Shaker water bath.—Maintaining 70°–80°C. C14:1-9-tetradecenoic methyl es ter, C 15:0-pentadecanoic methyl
(i) Steam bath.—Supporting common glassware. ester, C15:1-10-pentadecenoic methyl es ter, C 16:0 -hexadecanoic
(j) Water bath.—With nitrogen stream supply, maintaining 40° ± m e t h y l  e s t e r ,  C 1 6 : 1 - 9 - h e x a d e c e n o i c  m e t h y l  e s  
t e r,
5°C. C17:0-heptadecanoic methyl es ter, C 17:1-10-heptadecenoic methyl
ester, C18:0-octadecanoic methyl es ter, C 18:1-9-octadecenoic methyl
(k) Wrist ac tion shaker. —Designed for Mojonnier cen trifuge
e s t e r , C 1 8 : 2 - 9 , 1 2 - o c t a d e c a d i e n o i c  m e t h y l  e s   t e r,
baskets.
C18:3-9,12,15-octadecatrienoic methyl es ter, C20:0-eicosanoic methyl
(l)rpm.
600 Mojonnier mo tor driven cen trifuge.—Optional; maintaining ester, C20:1-8-eicosenoic methyl es ter, C 20:2-11,14-eicosadienoic
methyl es ter, C 20:3 -11,14,17-eicosatrienoic methyl es ter, and
(m) Gravity convection oven.—Maintaining 100° ± 2°C. C22:0-docosanoic methyl es ter. Pre pare in dividual FAME stan dard
(n) Vortex mixer. solutions as fol lows: Break top of glass vial open and care fully
(o) Gas dispersion tubes.—25 mm, po rosity “A,” ex tra coarse, 大咖免
transfer contents to 3-dram glass vial. Wash origi  nal vial with hexane 费礼包
175 mm. to en sure com plete trans fer and add washings to 3-dram glass vial.
(p) Three-dram vi als.—About 11 mL. Add 1.0 mL C11:0 FAME standard solution, (2), dilute to total volume
(q) Phenolic closed top caps.—With polyvinyl liner, to fit vials. of ca 3.0 mL with hex ane. In dividual FAME stan dard so lutions are 9.9元
抢会员
(r) Teflon/silicone septa.—To fit vials. tor (2°–8°C).
stable up to 1 week when stored in re frigera 
1
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Table 996.06A. Interlaboratory study re sults for determination of total fat in food by hydrolytic ex traction—gas chromatography

No. of labs/ 0 下载券 加入VIP

Product
a
x, % outliers sr 1 /5 sR r
b
R
c RSDr, % RSDR, % HorRat
Wheat-based cereal 1.96 — 0.208 0.260 0.582 0.728 10.6
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3.69
Peanut butter 46.3 10/2 0.86 2.37 2.41 6.64 1.85 5.12 2.28
Fish sticks 11.2 10/2 0.354 0.541 0.991 1.51 3.14 4.80 1.73
Parmesan cheese 26.5 — 0.540 4.17 1.51 11.7 2.04 15.8 6.47
Chocolate cake (baked) 13.3 — 0.929 1.95 2.60 5.46 7.00 14.7 5.43

Fruit snack 3.92 10/1 0.087 0.146 0.244 0.409 2.22 3.74 1.15
Ground beef 21.9 10/1 1.11 1.82 3.11 5.10 5.06 8.32 3.31
Yogurt 1.46 — 0.131 0.222 0.367 0.622 8.98 15.2 4.03
a
Blind duplicates.
b
r = 2.8 ´ sr.
c
R = 2.8 ´ sR.

D. Extraction of Fat  
( b ) Dairy prod u cts. —Ac cu rately weigh ground and
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Finely grind and homoge 
nize test samples prior to extraction of fat. homoge  nized test por tion (con taining ca 100–200 mg fat) into
labeled Mojonnier flask. Force material into flask as far as possible. 鱼油的
[Note: With ma trixes of un known com position, it may be
Add ca 100 mg pyrogallic acid, C(a), and 2.00 mL triglyceride
necessary to analyze test portion without addition of internal
internal standard solution, C(l). Add a few boiling granules to flask.
standard to ensure against interferences. Should interfering peak be
Add 2.0 mL eth a  nol and mix well un til en tire test por tion is in
found, the area of C 11 in ternal stan dard peak must be cor rected
solution. Add 4.0 mL H2O and mix well. Add 2.0 mL NH4OH, C(c),
before performing calculations. Use 2.0 mL chloroform instead of
and mix well. Place flask into bas ket in shak ing wa ter bath at

internal standard solution.]
(a) Foods ex cluding d airy prod ucts and cheese. —Accurately
weigh ground and ho moge  nized test por tion (con tain ing ca
100–200 mg fat) into la beled Mojonnier flask. Force ma terial into
flask as far as pos sible. Add ca 100 mg pyrogallic acid, C(a), and
2.00 mL triglyceride in ternal stan dard so lution, C(l). Add a few
boiling gran ules to flask. Add 2.0 mL eth an ol and mix well un til
entire test por tion is in so lution. Add 10.0 mL 8.3M HCl and mix
well. Place flask into basket in shaking water bath at 70°–80°C set at
moderate agi  tation speed. Maintain 40 min. Mix contents of flask on
Vortex mixer ev ery 10 min to in corporate particulates ad hering to
sides of flask into solution. After digestion, remove flask from bath
and al low to cool to room tem pera  ture (20 °–25°C). Add enough
etha 
nol to fill bot tom reservoir of flask and mix gently.
70°–80°C set at mod erate ag i  tation speed. Main tain 10 min. Mix
contents of flask on V ortex mixer ev ery 5 min to in corporate
particulates adhering to sides of flask into solution. After digestion,
re move flask from wa ter bath and add a few drops of
phenolphthalein. Keep so lution ba sic (pink) with ad dition of
ammonium hydroxide. Add enough ethanol to fill bottom reservoir
of flask and mix gently.
(c) Cheese.—Accurately weigh ground and homogenized test
portion (con taining ca 100–200 mg fat) into la beled Mojonnier
flask. Force ma terial into flask as far as pos sible. Add ca 100 mg
pyrogallic acid, C(a), and 2.00 mL triglyceride in ternal stan dard
solution, C(l). Add a few boil ing gran ules to flask. Add 2.0 mL
etha 
nol and mix well un til en tire test por tion is in so lution. Add
4.0 mL H2O and mix well. Add 2.0 mL NH4OH, C(c), and mix well.

 
Table 996.06B. Interlaboratory study results for de termination of saturated fat in food stuffs by hydrolytic ex traction—
gas chromatography

No. of labs/
Product
a
x, % outliers sr sR r
b
R
c RSDr, % RSDR, % HorRat
Wheat-based cereal 0.493 10/0 0.0391 0.0522 0.109 0.146 7.92 10.6 2.39
Peanut butter 8.72 10/1 0.257 1.81 0.720 5.07 2.95 20.7 7.18
Fish sticks 3.00 10/1 0.223 0.572 0.624 1.60 7.44 19.1 5.64
Parmesan cheese 17.4 — 0.311 2.46 0.871 6.89 1.79 14.1 5.42

Chocolate cake (baked) 3.56 — 0.171 0.304 0.479 0.851 4.81 8.55 2.59
Fruit snack 1.27 10/2 0.0242 0.0362 0.0678 0.101 1.90 2.83 0.74
Ground beef 9.98 10/1 0.636 1.39 1.78 3.89 6.38 13.9 4.92
Yogurt 0.986 — 0.119 0.170 0.333 0.476 12.1 17.2 4.30
a
Blind duplicates.
b
r = 2.8 ´ sr.
c
R = 2.8 ´ sR.

ã 2005 AOAC IN TERNATIONAL

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Table 996.06C. Interlaboratory study results for de termination of monounsaturated fat in food stuffs by hydrolytic ex traction—
gas chromatography

No. of labs/
Product
a
x, % outliers sr sR b
r R
c RSDr, % RSDR, % HorRat
Wheat-based cereal 0.280 — 0.0320 0.0560 0.0896 0.157 11.4   20.0 4.14
Peanut butter 22.3 10/2 0.411 1.11 1.15 3.11 1.84 4.96 1.98
Fish sticks 1.83 — 0.165 0.313 0.462 0.876 9.02 17.1 4.69
Parmesan cheese 6.43 10/1 0.271 1.09 0.759 3.05 4.20 17.0 5.63
Chocolate cake (baked) 3.79 — 0.413 1.27 1.16 3.56 10.9 33.5 10.25

Fruit snack 1.08 10/2 0.0453 0.734 0.127 2.06 4.17 67.7 17.16
Ground beef 8.88 — 0.930 1.96 2.60 5.49 10.5 22.0 7.65
Yogurt 0.345 10/1 0.0222 0.0542 0.0621 0.152 6.42 15.1 3.23
a
Blind duplicates.
b
r = 2.8 ´ sr.
c
R = 2.8 ´ sR.

Place flask into bas ket in shak ing wa ter bath at 70 °–80°C set at
moderate agi  tation speed. Maintain 20 min. Mix contents of flask on
Vortex mixer ev ery 10 min to in corporate particulates ad hering to
sides of flask into so lution. Add 10.0 mL 12M HCl and place flask
into boil ing steam bath and main tain 20 min. Mix flask con tents
every 10 min using Vortex mixer. Remove flask from steam bath and
allow to cool to room tempera  ture (20°–25°C). Add enough etha  nol
to flask to fill bot tom reservoir and mix gently.
(d) Extraction.—Add 25 mL di ethyl ether to Mojonnier flask
from (a), (b), or (c). Stopper flask and place in cen trifuge bas ket.
Place bas ket in wrist ac tion shaker, se curing flask in shaker with
rubber tub ing. Shake flask 5 min. Rinse stop per into flask with
diethyl ether–petroleum ether mixture, C(k). Add 25 mL
petroleum ether, stop per flask, and shake 5 min. Cen trifuge flask
(in basket) 5 min at 600 rpm. (Note: If centrifuge is not available,
al low
stop percon tents
into to set
flask withatdi
least 1 h un
ethyl til upper
ether–pe trolayer
leum is clear.)
ether mixRinse
ture.
Decant ether (top) layer into 150 mL beaker and carefully rinse lip
of flask into beaker with di ethyl ether–pe troleum ether mix ture.
Slowly evapo  rate ether on steam bath, using nitrogen stream to aid
in evaporation. Residue remaining in beaker contains extracted fat.
E. Methylation
F. GC Determination
Rela  tive re tention times (vs FAME of triglyceride in ternal
standard solution) and response factors of individual FAMEs can be
obtained by GC analysis of individual FAME standard solutions and
mixed FAME stan dard so lution. In ject ca 2 mL each of in dividual
FAME stan dard so lutions and 2 mL of mixed FAMEs stan dard
so lu tion. Use mixed FAMEs stan dard so lu tion to op ti mize
chromatographic response before injecting any test solutions. After 猜你喜
all chromatographic conditions have been optimized, inject test
solutions from E. 鱼油的
G. Calculations
Total fat is the sum of fatty acids from all sources, expressed as
triglycerides. Expressing measured fatty acids as triglycerides
requires mathematical equivalent of condensing each fatty acid
with glyc erol. For ev ery 3 fatty acid mol e  cules, 1 glyc erol
(HOCH 2CHOHCH 2OH) is re quired. Es sentially, 2 meth y   lene
groups and 1 methine group are added to ev ery 3 fatty ac ids.
Calculate re tention times for each FAME in in dividual FAMEs
standard solutions, C(m)(3), by sub tracting re tention time of C 11:0
peak from re tention time of fatty acid peak. Use these re tention
times to iden tify FAMEs in mixed FAMEs stan dard so lution. Use
ad di tional FAME so lu tions (from the same sup plier) when
necessary for complete FAME identity verification.

Dissolve extracted fat resid ue in 2–3 mL chloroform and 2–3 mL (a) Calculate response factor (Ri) for each fatty acidi as follows:
diethyl ether. Trans fer mix ture to 3 dram glass vial and then Ps i W C11:0
evapo rate to dryness in 40°C water bath under nitrogen stream. Add Ri = ´
Ps C11:0 Wi
2.0 mL 7% BF 3 re agent, C(j), and 1.0 mL to luene, C(g). Seal vial
with screwcap top con taining Tef lon/sili 
cone sep tum. Heat vial in
oven 45 min at 100°C. Gently shake vial ca ev ery 10 min. ( Note: where Psi = peak area of in dividual fatty acid in mixed FAMEs
Evaporation of liquid from vials indicates inadequate seals; if this standard solution; PsC 11:0 = peak area of C 11:0 fatty acid in mixed
occurs, discard solution and repeat the entire procedure.) Allow vial FAMEs standard solution; WC11:0 = weight of in ternal stan dard in

to cool to room tempera  ture (20°–25°C). Add 5.0 mL H2O, 1.0 mL mixed FAMEs
FAME in mixedstan dard so
FAMEs ludard
stan tion; so
and Wi = weight of in dividual
lution.
hexane, and ca 1.0 g Na2SO4, C(i). Cap vial and shake 1 min. Allow
layers to sepa 
rate and then carefully transfer top layer to another vial (Note: Peaks of known iden tity with known rel a  tive re tention
containing ca 1.0 g Na 2SO4. ( Note: Top layer con tains FAMEs times are listed in Table 996.06D. When peaks of unknown identity
including FAME of triglyceride internal standard solution.) are ob served dur ing the chro matographic run, at tempt to iden tify
such peaks us ing MS, FTIR, etc. Peaks of unkown iden tity should
Inject FAMEs onto GC column or transfer to autosampler vial for not be in cluded in the sum mation when quan tifying fat in the test
GC analysis. portion.)

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