Sucralose, also known as sucralose, commonly known as sucralose, is a new type of sweetener developed by Tate & Lyie and the University of London and patented in 1976. Because it has high sweetness (600 times sweetness of sucrose) and pure sweetness, it is considered to be one of the best functional sweeteners at present, representing the highest level of research on powerful sweeteners. Although scientists have demonstrated high safety through long-term toxicological experiments, there are also reports that sucralose can induce episodes of migraine.
Establishing a method for determining sucralose in food can provide productive guidance for food production enterprises and provide food quality supervision basis for quality supervision departments. China's national standard "GB 22255-2014 National Food Safety Standard Determination of Sucralose (Sucralose) in Foods" has established a HPLC-ELSD detection method for sucralose.
Method advantages:
Based on the national standard “GB 22255-2014 Food Safety National Standard Food Determination of Sucralose (Sucralose) in Foodsâ€, Dima Technology has optimized the method and introduced the “Measurement of Sucralose in Food†method. :
Determination of sucralose in food by solid phase extraction-high performance liquid chromatography, purification of the sample by ProElut PLS solid phase extraction column, by HPLC-ELSD;
The pre-treatment steps are simple, the purification effect is good, and the reproducibility is good. The limit of quantification is 7.5 mg/kg, which is in line with the GB 22255-2014 national food safety standard. Determination of sucralose (sucralose) in foods. ;
Applicable to all provinces and cities for entry and exit, quality inspection, disease control, food and drug inspection, third-party testing institutions, food testing institutions, large food producers, universities and research institutes.
The following is a detailed solution, please refer to!
Determination of sucralose in foods - HPLC method
1. Scope of application
This program is suitable for the detection of sucralose in liquid milk, yogurt, soy sauce, vinegar, biscuits, cheese, milk tea, cola and jelly. The method has a limit of 7.5 mg/kg.
2, standard preparation
Standard stock solution: accurately weigh the standard, prepare 10 mL/mL stock solution with water, and draw a certain volume of 10 mg/mL stock solution into a stock solution with a concentration of 1000 μg/mL.
3, extraction
3.1 Protein-containing fat liquid: liquid milk, yogurt, soy sauce and vinegar
10 mL sample, add 8 mL water and 2 mL 200 g / L lead acetate solution, shake for 2 min, ultrasonic extraction for 5 min, centrifuge at 6000 rpm for 5 min, take 10 mL of supernatant, to be purified;
3.2 Protein-containing fat solids: biscuits, cheese and milk tea
5 g sample, add 8 mL water and 2 mL 200 g / L lead acetate solution, shake for 2 min, ultrasonic extraction for 5 min, centrifuge at 6000 rpm for 5 min, take 10 mL of supernatant, to be purified;
3.3 Beverage: Coke (pre-sounding ultrasonic bubble)
10 mL sample, add 10 mL water, mix, take 10 mL, to be purified;
3.4 Jelly
5 g sample, add 5 mL of water, dissolve in hot water, mix well, and purify.
Note: The extract of GB 22255-2014 National Food Safety Standard for Determination of Sucralose (Sucralidin in Food) is a 75% methanol aqueous solution. During the concentration process under reduced pressure, the boiling point is severe and difficult to operate.
4, purification - ProElut 200 mg / 6 mL PLS (Cat. #:68012)
(1) Activation:
Add 5 mL of methanol and 5 mL of water to the column in turn, and discard the effluent;
(2) Loading:
Add the liquid to be purified to the column and discard the effluent (control flow rate does not exceed 1 drop per second);
(3) rinsing:
(4) Elution:
Add 5 mL of 20% aqueous methanol to the column and discard the effluent;
Add 3 mL of methanol to the column and collect the effluent;
(5) Constant volume:
The eluate was evaporated to dryness under reduced pressure at 50 ° C and then taken to 1 mL with mobile phase for HPLC analysis.
5, chromatographic conditions
Column: Diamonsil C18(2) 150 × 4.6 mm, 5 μm (Cat.#:99601)
Flow rate: 1.0 mL/min
Injection volume: 20 μL
Column temperature: 35 °C
Detector: SEDEX LT-ELSD, temperature: 40 ° C, pressure: 3.5 bar, Gain: 6
Mobile phase: A: water; B: acetonitrile
Gradient setting
Time / Min.
0
14
15
twenty two
twenty three
30
A (%)
89
89
10
10
89
89
B (%)
11
11
90
90
11
11
6, add recycling results
Addition and recovery results of HPLC detection of sucralose in food
Add level 200 mg/kg
Add level 20 mg/kg
Add level 7.5 mg/kg
Blank content (μg/mL)
Recovery rate(%)
Scaling amount
Recovery rate(%)
Scaling amount
Recovery rate(%)
Scaling amount
Breakfast milk
99.01
10 mg/mL 200 μL
109.82
1000 μg/mL
200 μL
96.52
1000 μg/mL
75 μL
-
Chocolate milk
99.70
10 mg/mL 200 μL
100.91
1000 μg/mL
200 μL
95.88
1000 μg/mL
75 μL
-
Coffee milk
100.34
10 mg/mL 200 μL
112.34
1000 μg/mL
200 μL
126.00
1000 μg/mL
75 μL
-
Yakult
128.83
10 mg/mL 200 μL
-
-
-
-
130.8
Yogurt
-
-
105.58
1000 μg/mL
200 μL
123.42
1000 μg/mL
75 μL
-
soy sauce
77.85
10 mg/mL
200 μL
-
-
-
-
113.48
vinegar
108.22
10 mg/mL
200 μL
143.64
1000 μg/mL
200 μL
205.47
1000 μg/mL
75 μL
-
Biscuits
-
-
102.64
1000 μg/mL
100 μL
103.28
1000 μg/mL
37.5 μL
-
cheese
-
-
88.04
1000 μg/mL
100 μL
82.78
1000 μg/mL
37.5 μL
-
Milk tea
-
-
101.48
1000 μg/mL
100 μL
169.05
1000 μg/mL
37.5 μL
-
Cola
-
-
103.97
1000 μg/mL
200 μL
98.49
1000 μg/mL
75 μL
-
jelly
-
-
93.89
1000 μg/mL
100 μL
96.27
1000 μg/mL
37.5 μL
-
Determination of sucralose in foods - HPLC method related product information:
Item number
name
specification
Sample preparation
68012
ProElut PLS
200 mg/6 mL, 30/pk
244358
12 tube anti-cross-contamination vacuum SPE extraction device
12 digits
4803
1,3,6mL column tube universal connector
15/pk
4806
Cooke (control flow)
15/pk
99011
Vacuum/positive pressure dual purpose pump, no oil
1/pk
99013
Filter bottle set
(including silicone rubber tube 2 meters, 2L suction filter bottle and rubber stopper)
1/pk
30039
FitMax needle filter Nylon
13 mm, 0.22 μm 100/pk
30040
FitMax needle filter Nylon
13 mm, 0.45 μm 100/pk
Standard
53-69293-100G
Sucralose [56038-13-2]
100 g
Column and guard column
99601
Diamonsil C18(2)
150 × 4.6 mm, 5 μm
HPLC Solvent? Buffer Salt? Ion Pair Reagent
50101
Acetonitrile HPLC grade
4 L
50102
Methanol HPLC grade
4 L
General purpose chromatography products
52401B
Bottle holder / blue (spot)
50 holes
52401A
Bottle holder / white (spot)
50 holes
1034
Vial (brown/thread)
2 mL, 100/pk
1035
Sample cap/with pad (already assembled)
100/pk
H80465
HPLC syringe
25 μL
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