Konservantide (bensoehappe ja sorbiinhappe) määramine

Aura active mahlajoogist HPLC meetodil

RT A H C (mg/l)
Bensoeh. Sorbiinh. Bensoeh. Sorbiinh. Bensoeh. Sorbiinh. BH SH 1.40E+04
Stdl. 1 7.43 10.50 1.30E+04 ### ### 4.85E+04 8.110 2.48
1.20E+04 f(x) = 1572.2672898522 x + 272.467837
Stdl. 2 7.54 10.62 8.97E+03 ### ### 3.30E+04 5.407 1.65 R² = 0.99846539132845
Stdl. 3 7.45 10.49 6.47E+03 ### ### 2.35E+04 4.055 1.24
Stdl. 4 7.44 10.47 3.49E+03 ### ### 1.89E+04 2.028 0.62 1.00E+04
Proov 1 7.43 8.29E+03 ###
8.00E+03
Proov 2 10.43 ### 4.65E+04
6.00E+03
Regressioonanalüüs:
4.00E+03
Bensoehape Sorbiinhape
b1= 1572.267 272.4678 =b0 b1= 7755.415 -733.1428563 =b0 2.00E+03
s(b1)= 43.58567 234.2683 =s(b0) s(b1)= 40.70718 75.870994702 =s(b0)
r2= 0.998465 192.5978 = S r 2= 0.999972 36.347527872 = S 0.00E+00
0.000 2.000 4.000 6.000 8.000 10.000
Konts. lahjendusel (mg/l): Konts. joogis (mg/l):
CBH= 5.099344 CBH= 101.9869
CSH= 2.429676 CSH= 145.7805

* Bensoehappe määramiseks tegin Aura joogist 20x lahjenduse, 2.00E+04

sorbiinhappe määramiseks aga 60x lahjenduse.
1.80E+04 f(x) = 7755.41474632824 x − 733.14285
1.60E+04 R² = 0.999972450095769
Residuaalid: 5.36E+01 3.04125 ### 0.98167
BH: ### 0.33792 SH: 2.91E+01 0.15500 1.40E+04
1.74E+02 -1.01375 ### -0.25833 1.20E+04
### -3.04125 ### -0.87833
1.00E+04
8.00E+03
Cs 8.11 mg/l 6.00E+03
teg 0.05 mg/l
4.00E+03
temp 0 mg/l
0.05 mg/l 0.00617 2.00E+03
0.00E+00
V100 100 ml 1.00 1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60
kal 0.01 ml
täit 0.0519615
temp 0
0.052915 0.00053

Vautom.pip. 5000 μl 0.0034641 6.93E-07

2500 μl 0.0069282 2.77E-06
1000 μl 0.0034641 3.46E-06

CBH 5.099344 mg/l

Aa ###
Ha ###
süst 0.2 % 192.598 mAu·s
vool 0.3 % 0.000 mAu·s
kord 0.02 mAU 0.000 mAu·s
Integr 2.5 % 119.656 mAu·s
triiv 0.1 mAU/h 0.038 mAu·s
uc(Aa)= 226.741 mAu·s
b0, b1 u(b0,b1)= 96.689 mAu·s

u(CBH(lahj), proov)= 0.144 mg/l 0.02828

u(CBH(lahj), regr)= 0.061 mg/l 0.01206
u(CBH(lahj))= 0.157 mg/l

uc(CBH), suht = 0.031

uc(CBH)= 3.198
Tulemus:
CBH= 102 mg/l
u(CBH)= 6 mg/l k=2 (norm)

Cs 2.48 mg/l
teg 0.05 mg/l
temp 0 mg/l
 0.05 mg/l 0.02016
CSH 2.429676 mg/l
Aa ###
Ha ###
süst 0.2 % 36.348 mAu·s
vool 0.3 % 0.000 mAu·s
kord 0.02 mAU 0.000 mAu·s
Integr 2.5 % 261.395 mAu·s
triiv 0.1 mAU/h 0.045 mAu·s
uc(Aa)= 263.910 mAu·s
b0, b1 u(b0,b1)= 30.950 mAu·s

u(CSH(lahj),proov)= 0.034 mg/l 0.01401

u(CSH(lahj),regr)= 0.004 mg/l 0.00164
u(CSH(lahj))= 0.034 mg/l

uc(CSH),suht= 0.025
uc(CSH)= 3.588

Tulemus:
CSH= 146 mg/l
uc(CSH)= 4 mg/l k=2 (norm)
 BH:

1.40E+04

1.20E+04 f(x) = 1572.2672898522 x + 272.467837637

R² = 0.99846539132845
1.00E+04

8.00E+03
Column D
Linear
6.00E+03 (Column D)

4.00E+03

2.00E+03

0.00E+00
0.000 2.000 4.000 6.000 8.000 10.000

SH:

2.00E+04
1.80E+04 f(x) = 7755.41474632824 x − 733.14285632939
1.60E+04 R² = 0.999972450095769
1.40E+04
1.20E+04
Column E
1.00E+04 Linear
8.00E+03 (Column E)
6.00E+03
4.00E+03
2.00E+03
0.00E+00
1.00 1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60
Teoreetiliste taldrikute arv

2 BH SH
tr tr(cm)=

()
10.05 14.1
N=5,54 w1/2(cm)= 0.4 0.45
w1 N= 3497.21156 5439.04889
k'= 1.3372093 2.27906977
2
As= 1.66666667 2.16666667

Analüüdi mahtuvusfaktor: Rs= 5.60553633

α= 1.70434783

tr −t M
k '=
tM tM= 4.3

Asümmeetriafaktor: Lahutuvuskriteerium:

w2 t r (BH )−t r( SH )
A s= Rs =
w1 0 , 85⋅(w1 /2 (BH )+w1 /2( SH ) )
Selektiivsusfaktor:

k ' SH
α=
k ' BH
k' väärtus BH piigi korral on normaalne, SH puhul väga hea.
As puhul loetakse normaalseks väärtuseks <2.
N puhul oleks hea, kui väärtused oleksid üle 10000,
aga antud juhul on meil seda raske saavutada.
Piigid loetakse lahutunuks, kui Rs>1,5