Xây dựng quy trình định lượng acid propionic trong một số thực phẩm bằng phương pháp sắc ký lỏng hiệu năng cao

BỘ GIÁO DỤC VÀ ĐÀO TẠO BỘ Y TẾ















































































720410



   khoa  









 y . 



- 

              
 
                

Hà Nội, ngày 30 tháng 8 năm 2013
 viên






AOAC (Association of Official Analytical
Chemists)

AP
Acid Propionic
ATVSTP

GC/FID (Gas chromatography with hydrogen
flame ionization detector)

HPLC (High performance liquid
chromatography)

LOD (Limit of Detection)

LOQ (Limit of Quantification)

MeCN
Acetonitil
MeOH
Methanol
PA

QC (Quality control)


SAX (Strong anion exchange)

SPE (Solid phase extraction)

TCVN



Trang
 
7

32

34

35

38

40

41

43

45

46
AP trong nhóm bánh

49
AP 
50

53

55

56

57

59








Trang

16
Hình 1.2AP 
17

24
Hình 3.4: Ph
29

Hình 3.5
33
Hình 3.6
35
Hình 3.7
36
Hình 3.8
36
Hình 3.9
37
Hình 3.10
38
Hình 3.11: 
39
Hình 3.12: 
40
: opionic
42
:  AP
42
0 ppm
47

47
Hình 3.17 
48

51
Hình 3.19
51

Hình 3.20
52
.21
53

54
Hình 3.23
58
Hình 3.24
58



1.  Hóa phân tích I
2.  Hóa phân tích II, tr. 123-
3. 

4. 
5. --BYT q
 .
6. - 

.
7.      ),      

8. 
.
9.   .    

.

10.    
, 
tr.1-8.
11. Khoai Tây (2012),       
tháng 04, tr.38.
12. TCVN ISO/IEC 17025:2005, 

13. 
, N
14. , 

15. 
, 



16. Ackemans M. T., Ackermans  Loonen J. C. J. M. and Beckers J. L. (1992),
        
Journal of Chromatography, 627, pp. 273-279.
17. Amit Keshav, Kailas L. Wasewar, Shri Chand (2009)Recovery of Propionic acid
by reactive extraction -1. Equilibrium, effect of pH and temperature, water
Desalination and water treatment, Vol.3, p.p 91-98.
18. AOAC International (2007), How to meet ISO 17025 requirements for method
verification, USA.
19. AOAC official method 950.35 (2000), Acetic and Propionic acids in bread/cakes-
Chromatographic method may also be referred as alternative method.
20. Beljaars, PRDijk, R.van, Verheijen, PJJ, Anderegg (1996)
determination of propionic acid and sorbic acid contents of rye bread:
, Journal of AOAC International, vol.79 (4).
21. Biyang Deng (2008), "Quantitative analysis of propionic acid in bread by capillary

electrophoresis methods", Journal of Pharmaceutical and Biomedical Analysis,
p.1249-1253.
22. Cao Ye (2005), A determination of propionic acid type antimicrobial preservatives
of feed by HPLCSouthwest China Journal of Agricultural Sciences, Vol. 18
(1), pp. 111-112.
23. Carlos Ibáñez  Analysis of total propionic acid in feed using headspace
solid-phase microextraction and gas chromatography, Journal of
Chromatography A, Vol. 1017, pp. 161-166.
24. Eiichi Ishikuro, Hiroshi Hibino, Tomoyoshi Soga, Hiroko Yanai, Hirokazu Sawada
        
 Journal of the food hygenic society of Japan, vol. 41(4),
pp.261.
25.           
efficacy of Propionic acid, Sodium propionate, Calcium propionate and
EFSA Journal 2011, vol.9 (12),
pp.2446.
26. Federal Agency for the safety of the food chain (2012), Determination of Propionic
acid, France.
27. Food safety and standards authority of India Ministry of Health and family welfare
Government of India (2012), Food additives, pp.40-41, New Delhi.
28. Hen Sebbag, Joachim Weiss, Zamir Manor, Olga Goldberg Oster, Yeoshua
Nachmani, Eitan JC Borojovich  Analysis Of Propionic And Acrylic
Acids By Reversed Phase HPLC With Anion Suppression And Conductivity
Analytica Chimica Acta, vol.551, pp.158 -169.
29. Japan Official method (2006), Determination of propionic acid, Calcium
propionate, Sodium propionate in food by Gas Chromatography.
30. Khaldun M. Al Azzam, Bahruddin S., Noor Hasani Hashim., Afidah Abdul Rahim.
       es and
        International
Food Research Journal, vol.17, pp.1107-1112.

31.            -
Chromatographic determination of Propionic acid added as a preservative to
Cereal Chemistry, Vol. 62 (1), pp.6-11.
32. Leo M.L. Nollet, Fidel Toldra (2012), Food analysis by HPLC, pp.534 Taylor and
Francisgroup, USA.
33. Scotter M. J. , Thorpe S. A. , Reynolds S. L. , Wilson L. A. & Strutt P. R. , (1994),
A rapid capillary gas chromatographic method for the determination of
propionic acid and propionates in bread and bread products Journal Food
Additives and Contaminants, Volume 11, Issue 3, May 1994, pp. 295-300.
34. Shibata Masato, Fujiwara Koki, Yamata Toshiaki (1999), Determination of
Propionic acid, Calcium propionate and Sodium propionate in Mixed Feed by
High Performance Liquid ChromatoraphyJournal of Chromatography A, (24),
pp. 79-90.
35. Shimazu (2005), Analysis Guidebook Food Product Analyses, pp.31.
36. Tateishi Yukinari, Nakazato Mitsuo, Ushiyama Hirofumi, Kobayashi Chigusa,
        
        
Annual Report of Tokyo Metropolitan Research Laboratory of Public Health,
No.49, pp.77-83.
37. Thailand National Bureau of Agricultural Commodity and Food Standards (2003),
- 
Compendium of method for food analysis, Issue 1, page 40-41.
38. Zhao JC, Guo ZA, Chang JH, Wang WJ (2001), “Study on reversed-phase high
performance liquid chromatography separation condition and determination
Chinese journal of Chromatography, 19(3), pp.260-
326.

Trang Web
39. Material Safety Data Sheet Propionic acid MSDS,
[www.sciencelab.com/msds.php?msdsId=9927407],  14/08/2012.

40. Propionic Acid[ />acid.aspx], ng
41. 
[ />80105d3f.pdf?filepath=productsafety/pdfs/noreg/23300419.pd &fromPage=Get
Doc




 GVHD: TS. 
2013

H





 1
1.  3
1.1. B 3
 3
1.1.13] 3
 3
1.1.2.2. Nguyên nhân bên ngoài 4
 5
 5
 8
 9
 10
 12

 12
 13
 13
 14
 15
 15
 15
1. 16
cid Propionic 17
1.3. C
 18
1. 18
 GVHD: TS. 
2013

H

 19
 20
 22
 22
 22
 22
 23
  23
 23
 24
 [6], [8] 24
 25
 25

2.3.2.2.  25
 25
 25
 26
2.3.3.3.  26
2.3.3.4.  26
) 27
2.3.3.7 27
 27
2.3.5 27
 29
3.1.
29
3.1.1.  29
3.1.2.  29
3. 30
3.1.4.  30
 GVHD: TS. 
2013

H

3. 31
 31
 31
 31
 32
 33
 34
 34

 35
 37
 37
 38
 39
 39
 40
 41
 44
 48
-  52
 54
 55
 60
 60
 61
 61
 63


 GVHD: TS. 
2013

 Page 1


 m quan
  . Nó góp

  m. C           

  
     ngày
nay ngày càng 
ích,
 công

Acid Propionic là c          
.   
vào 


13]. Tuy nhiên, n
 m lâu
 

[25], [39]. -BYT, gcho phép 
  
  
. acid Propionic  

5].


 GVHD: TS. 
2013

 Page 2

         






pháp 
.
Tuy nhiên,     ,      c phân tích

 acid Propionic trong  
 

 quy trình phân tích acid Propionic 

 
 










 GVHD: TS. 
2013

 Page 3

. 
1.1. B
1.1.1. 








(

.






1.1.2 [13]
1.1.2.1. Nguyên nhân nội tại
 
 



 GVHD: TS. 
2013

 Page 4




 



1.1.2.2. Nguyên nhân bên ngoài


.

-Clostridium, Bacillus, Proteus, Pseudomonas,
Streptococcus
-       Pseudomonas, Achromobacter,
Micrococ
- 
- 
+ Serratia marcescens, Micrococcus roseus

+ Pseudomonas flourescens, Flavobacterium, Micrococcus flavus làm cho

+ Pseudomonas nigrifaciens 
-             Alcaligenes
viscolactis.
- 

 GVHD: TS. 

2013

 Page 5

-  :
Bacillus Subtilis, Bacillus mesentericus, Bacillus megaterium 



lên men các 
 Saccharomyces        Pichia, Hansenula,
Debaryomyces            Pichia,
Hansenula Debaryomyces
      Candida mycoderma      



 . Penicillium,    

Asper
 


a môi





1.1.3 [11],[13]

1.1.3.1. Bảo quản ở nhiệt độ thấp

 GVHD: TS. 
2013

 Page 6





them Clo (40-


 



0

-1
0
C.
 


    
3
. CH
3

Cl, CO
2
, SO
2
, F
2
, CCl
2
F
2
     

             

0

0
-
                 
-1
0
-2
0
-3
0
C


  -   



 

 GVHD: TS. 
2013

 Page 7

1.1: 
TT


0
C

1

8-15
Tháng-
2
Chè
10
Vài tháng
3

- 
2  5
(-10)  (-18)
1 - 2 ngày
3 tháng

4

2-6
1 - 3 ngày
5

2  6
1  3 ngày
6

- 
2  5
(-10)  (-18)
2  3 ngày
2  3 tháng
7


3 ngày
8

- 
2  5
(-10)  (-18)
2  3 ngày
2 tháng
9

- 
2  5

(-10)  (-18)
2  3 ngày
2  3 tháng
10

- 
2  5
(-10)  (-18)
1  2 ngày
2  3 tháng
11

5  8
4  
12
chin
- 
5  8
0  7
< 7 ngày

13

0  7
7  14 ngày
14

1  7
5  7 ngày
15


2  7
6 tháng

 GVHD: TS. 
2013

 Page 8


    -18
0
 
-40
0
-50
0
C v
nhanh.

-15
0
-20
0
-12
0
C
-15
0
-





1.1.3.2. Bảo quản ở nhiệt độ cao



0

0
 

     
0
C



0

0

-


0

0



0


              

 GVHD: TS. 
2013

 Page 9


v-75
0
C trong vòng 15-20 giây,
,7
0


 

0
-38
0
C trong 2-3


0
-12
0



       

1.1.3.3. Bảo quản bằng phương pháp làm khô




n







 


0
C, quay 18-

0


 GVHD: TS. 
2013

 Page 10






-90
0


* Dùn


-60
0

h



1.1.3.4. Áp dụng sức thẩm thấu để bảo quản



-
s


 


                
Clostridium botulinum