
TRƢỜNG ĐẠI HỌC KHOA HỌC TỰ NHIÊN
Nguyễn Thị Hà Bình
XÁC ĐỊNH OCHRATOXIN
TRONG THỰC PHẨM BẰNG PHƢƠNG PHÁP
SẮC KÝ LỎNG KHỐI PHỔ (LC-MS/MS)

- 2013
1
LỜI CẢM ƠN

 
 


,
, 





 





Hà Nội, năm 2013


Nguyễn Thị Hà Bình
Luận văn thạc sĩ Nguyễn Thị Hà Bình
Luận văn thạc sĩ Nguyễn Thị Hà Bình 3
3.1 Tối ƣu các điều kiện chạy máy LC-MS/MS 23

3.1.1.1 Khảo sát ion mẹ và ion con.23
3.1.1.2 Tối ưu các điều kiện MS24
3.1.2 Tối ƣu các điều kiện chạy sắc ký lỏng hiệu năng cao (HPLC)……….26
3.1.2.1 Pha tĩnh………26
3.1.2.2 Khảo sát thành phần pha động.27
3.1.2.3 Khảo sát tốc độ pha động 29
3.1.2.4 Chọn chương trình chạy gradient…30
3.2 Tối ƣu quy trình xử lý mẫu3
3.2.1 Chọn quy trình xử lý mẫu………………………………………………33
3.2.2 Khảo sát thể tích (số lần chiết) dung môi chiết…………………… 36

 37
3.2.5 Khảo sát thể tích dung môi rửa giải………………………………….38
 38
3.3 Thẩm định phƣơng pháp phân tích2
3.3.1 Tính đặc hiệu / chọn lọc………………………………………………42
3.3.2 Giới hạn phát hiện (LOD), giới hạn định lƣợng (LOQ)………………44
3.3.3 Xác định khoảng tuyến tính……………………………………………45
3.3.4 Xây dựng đƣờng chuẩn
3.3.5 Độ chính xác (accuracy) của phƣơng pháp phân tích (độ đúng và độ
chụm) [9]………………………………………………………………………48
3.4 Phân tích mẫu thực tế
KẾT LUẬN VÀ KIẾN NGHỊ7
TÀI LIỆU THAM KHẢO 59

chromatography

IUPAC
International Union of Pure and
Applied Chemistry


LOD
Limit of detection

LOQ
Limit of quantity

MeOH
Methanol
metanol
MRL
Maximum Residue Limit

PSA
Primary and secondary amine

RSD
Relative standard deviation

SPE
solid phase extraction

IARC
International Agency for Research on

26

28

28

31

32

34
3.9 : 
36

37


37

38

42

45


46
6: 
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
29

30

30

32

35

40

41

43

43

44

46

47

47

48


- 
- 
- 
      





            

 

Luận văn thạc sĩ Nguyễn Thị Hà Bình 9
- 



 Mycoto

 


m . 
,  .   
,    cao. 



1.          Ochratoxin trong 
 
- 
Luận văn thạc sĩ Nguyễn Thị Hà Bình 10
- .
- 
ochratoxin trong  
 .

Luận văn thạc sĩ Nguyễn Thị Hà Bình 11
CHƢƠNG 1: TỔNG QUAN

1.1.Giới thiệu chung [14-15]
1.1.1.Định nghĩa
o 
            
              
             
 

 
 (
 

. Ochratoxins 

Ochratoxin A . Ochratoxin
A 
0


-1
OTA 
a1
= 4,2-4,
a2
= 7,0-
7,3. Ochratoxin A TLC)
.


221
0
C.
ochratoxins: ochratoxins 
ribonucleic axit (tA   s   
 - tA
 
               
tARN   ochratoxin A       
 ochratoxin A  
A

 A


-     

- 
, protein, 
Luận văn thạc sĩ Nguyễn Thị Hà Bình 14
             



 



            




heo: -6  mg/

1.1.3. Giới hạn tồn dƣ tối đa cho phép (MRL)
-        


Ochratoxin A 


  ochratoxin             
chratoxin- enzyme


    

    o          
ochratoxin           
Ochratoxin



, Lulu Feng, Ying Wang, Chenghua
He, Xichun Wang, Haibin Zhang [14

-
2,5-10 ppb. . 
 - 
, 
Luận văn thạc sĩ Nguyễn Thị Hà Bình 16
  Ochratoxin A   -23 ppb,       
Ochratoxin A -3 ppb.
     d Moulasa, Dua  
Prazeresb,  [32] 
n 
h  


  
-9 ppb, 
-90%.
27
2
c 
 . 
   , k     g    




1.2.4. Phƣơng pháp sắc ký lỏng khối phổ







-MS/MS

Luận văn thạc sĩ Nguyễn Thị Hà Bình 18



19
  

-NH
2
, -
n-

 
       C
18
H
37
      
methanol, axetonitr


          



  
            

                
cyclopentan, n-pentan, n-heptan, n-hexan, 2-chloropropan, cacbondisulfua
(CS
2
), chlorobutan, CCl

       

              



Detector







Luận văn thạc sĩ Nguyễn Thị Hà Bình 21
ionization             
chemical ionization  APCI).
a) Chế độ ion hóa đầu phun điện tử (ESI)




+
]
+

 
o 
o [M-H]
-
, [M-nH]
n-


          

b) Chế độ ion hoá hoá học ở áp suất khí quyển (APCI).

 


 

 Bộ phận phân tích khối



 
 - 







ring electrode
end-cap electrode


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