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Analysis of Sudans in Chilli powder Using Endeavorsil Columns

Method: HPLC-MS
Matrix: 0
Application No.: 101942
Componds: Sudan I, Sudan II, Sudan III, Sudan IV
Columns: Endeavorsil C18 1.8 μm 50 x 2.1 mm
Cat No.: 87002
Sample Pretreatment: Samples were obtained from a commercial source.
1. Weigh 1.0g of Chilli powder, add 10mL of acetone.
2. Vortex mixing for 20 min and then centrifuge for 5min at 12000rpm
4. 1mL aliquot of the supernatant solution is evaporated to dryness.
5. Add 1mL n-hexane to dissolve the residue for SPE cleanup.
6. SPE cartridge (DIKMA ProElut AL-B,500mg/3mL Cat# 65204)
The cartridge above is conditioned by 2mL methanol, 2mL ethyl acetate and 3mL n-hexane. Load sample solution onto the SPE cartridge. Wash it with 3mL hexane, 1mL 30:70 ethyl acetate/n-hexane.Elute with 8mL 50:50 ethyl acetate/methanol, collect the eluent, evaporate to dryness, then reconstitute in 0.4mL methanol with 4% ammonium.
Conditions: Mobile Phase: A: water
B: acetonitrile
Gradient: 70 to 100%B in 1.5min, hold6.5min, 100to 70%B in 0.1min, equilibrate at 70%B for 1.9 min
Scan mode: ESI+;
Flow Rate: 0.2mL/min;
Injection: 10µL;
Temperature: 20℃
Publisher: Dikma Technologies Inc.
Keyword: Sudans, Endeavorsil C18, Sudan I, Sudan II, Sudan III, Sudan IV
Abstract: Chilli powder samples with Sudans spiked are purified by AL-BSPE cartridge, then separated on DIKMA Endeavorsil columns for LC/MS/MS detection.

 

No.

Compounds

Retention Time(min)

Detection Ions

Concentration spiked(mg/kg)

Recovery (%)

LOD (µg/kg)

1

Sudan I

2.54

249.2>156.1*

249.2>128.1

2

98.3

1.5

2

Sudan II

3.28

277.2>121.2

277.2>156.1*

2

98.4

0.5

3

Sudan III

3.94

353.2>156.2

353.2>197.2*

2

99.6

2.5

4

Sudan IV

5.13

381.2>106.2

381.2>224.1*

2

90.2

1.0