Solid phase extraction method for detection of sulfonamides in animal-derived foods (SilibaseTM ALN)
First, the purpose of the experiment
In this experiment, solid phase extraction was used as a pretreatment method for samples, and LC-MS/MS method was used as a detection method. This method simplifies the pre-treatment of the sample and saves the amount of organic solvent.
Second, the experimental target
Sulfathiazole (CAS: 72-14-0), sulfamethazine (CAS: 127-79-7), sulfacetamide (CAS: 144-80-9), sulfapyridine (CAS: 144-83-2) , sulfamethoxazole (CAS: 127-69-5).
Third, the scope of application
The method is suitable for LC-MS/MS detection and confirmation of sulfonamides in animal-derived foods.
Fourth, the reference standard
Recommended National Standard GB/T 21316-2007 Determination of Sulfonamide Residues in Animal-derived Foods by Liquid Chromatography-Mass Spectrometry/Mass Spectrometry.
V. Experimental materials
SilibaseTM ALN solid phase extraction column 500mg/3mL.
Sixth, experimental methods
1, sample extraction
A 5 g sample will be weighed to the nearest 0.01 g. Place in a 50 mL vortex cap centrifuge tube, add 5 mL of water, and quickly mix for 1 min on a vortex mixer to completely dissolve the sample. Accurately add 15 mL of ethyl acetate, shake on a shaker for 10 min, centrifuge at 3000 r/min for 10 min, accurately pipette 12 mL of the upper layer of ethyl acetate into a 15 mL centrifuge tube, and place it in a concentrated nitrogen blower at 45 ° C to purify. Add 5 mL of water to dissolve and purify.
2, SPE column purification
The extract was passed through a neutral alumina column. After the solution was completely discharged, the column was washed with 2 x 3 mL of water, and then the column was rinsed with 5 mL of acetonitrile + water, and all the leachate was discarded. It was vacuum-dried with a vacuum pump for 10 min, and finally eluted with 6 mL of ethyl acetate. The eluent was collected in a 10 mL centrifuge tube, and dried at 45 ° C with a nitrogen purge. The volume was adjusted to 1 mL with acetonitrile + water (20 + 80). For LC-MS/MS on-board measurement.
3. LC-MS/MS conditions
Liquid chromatography-mass spectrometry/mass spectrometer
Column: C18 column: 150mm × 2.1mm, 2.0μm, or equivalent
Mobile phase: acetonitrile-0.1% formic acid
Seven, the experimental results
1, add recycling results
Different levels of tetracyclines were added to the samples, and the recovery results were as follows: (See Table 1)
Table 1 Results of tetracycline drug addition and recovery in animal tissues
| sample name | Compound name | Add level (ng/mL) | Recovery rate(%) |
| pork | Sulfathiazole | 50 | 84.76 |
| 100 | 89.44 | ||
| Sulfamethazine | 50 | 81.3 | |
| 100 | 91.08 | ||
| Sulfaacetamide | 50 | 92.92 | |
| 100 | 94.37 | ||
| Sulfapyridine | 50 | 81.74 | |
| 100 | 88.09 | ||
| Sulfamethoxazole | 50 | 81.81 | |
| 100 | 88.22 |
2, blank sample added pesticide residue chromatogram
Related Products
SilibaseTM ALN Solid Phase Extraction Column
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