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Experimental report on the determination of galactooligosaccharides

20231113-1067 Experimental report on the determination of galactooligosaccharides

Test Report

Chromatography conditions:

Column 

Welch Ultisil®HILIC Amide(4.6×150mm,3μm)

Mobile Phase

0.1% formic acid aqueous solution: acetonitrile

Column Temperature

30℃

Detector

UV

Injection Volume

10μL

Flow Rate

1.0 ml/min

Fluorescence detector

Excitation wavelength 355 nm, emission wavelength 430 nm

Elution procedure

Time (min)

Mobile phase A (%) 50 mmol/L

Ammonium formate, pH=4.4±0.1

Mobile phase B (%) acetonitrile)

0

2

98

7.50

2

98

8.00

16

84

16.00

16

84

50.00

39

61

51.00

80

20

54.00

80

20

55.00

2

98

70.00

2

98


Note

/

Chromatogram and Data: 

1) Blank solution detection spectrum

 Serial number 

Retention time (min)

Peak Area(mAU*min)

S/N

Relative peak area(%)

Resolution

(EP)

Number of plates(EP)

Asymmetry(EP)

Sum

 

0.000

 

0.00

0.00

 

 

2) Sample solution detection chart

 Peak name 

Retention time (min)

Peak Area

peak area(%)

Peak height

Resolution
(USP)

Tailing factor

Number of plates(EP)


20.030

42.03

0.30

1.99

 

 

 


20.790

76.03

0.55

 3.44 

 

 

 


21.609

35.27

0.26

1.80

 

 

 

 

22.461

13543.59

98.05

794.89

 

 

 

 

24.022

66.36

0.48

2.77

 

 

 

 

29.952

49.36

0.36

2.54

 

 

 

 

Sum

13812.63

 

 

 

 

 

 Peak name 

Retention time (min)

Peak Area

peak area(%)

Peak height

Resolution
(USP)

Tailing factor

Number of plates(EP)


19.944

39.57

0.29

1.90

 

 

 


20.702

73.07

0.54

3.28

 

 

 


21.524

34.44

0.25

1.73

 

 

 

 

22.374

13253.58

98.07

801.96

 

 

 

 

23.938

66.09

0.49

2.74

 

 

 

 

29.869

48.06

0.36

2.56

 

 

 

 

Sum

13514.82

 

 

 

 

 

3)Matrix curve (100 μg/mL)

Peak name 

Retention time (min)

Peak Area

peak area(%)

Peak height

Resolution
(USP)

Tailing factor

Number of plates(EP)


19.362

119.80

21.96

5.36

 

 

 


22.333

146.82

26.91

9.86

 

 

 


27.863

74.53

13.66

4.85

 

 

 

 

34.294

71.50

13.11

4.81

 

 

 

 

39.301

53.99

9.90

3.56

 

 

 

 

43.115

42.78

7.84

2.72

 

 

 

 

Sum

545.55

 

 

 

 

 

  • 4)Liquid mass spectrum (sample)

 



Conclusion:

Using Ultisil® HILIC Amide (4.6×150mm, 3μm), low-level oligosaccharides in powdered milk are detected. The peak profile of the standard sample matches the national standard, and qualitative analysis of the sample by liquid chromatography only detects maltose (2) at 461.17. This corresponds to the liquid chromatogram and meets the testing requirements.

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