In the liquid quality detection of veterinary drug residues in animal derived samples, lipid substances in the sample can interfere with the detection of the analyte. Lipids often form matrix enhancing or inhibitory effects on liquid quality detection, resulting in significant differences between the test recovery rate and the actual recovery rate of compounds, affecting the calculation of recovery rate and leading to significant deviations between test data and actual results.
Cleanert LipoNo is a newly developed degreasing material by Bonaire Technology Co., Ltd. The filler surface is modified with many long carbon chains, which can selectively adsorb fats. It uses QuEChERS to preprocess samples with high lipid content such as meat, eggs, milk, etc., which can ensure good recovery of veterinary drugs while removing lipids. The method is simple and convenient to operate, and is suitable for processing large amounts of samples.
Cleanert LipoNo is a large particle material that does not require centrifugation and can be layered by standing, further simplifying the operation.
Product Name |
Specifications |
Item number |
Cleanert LipoNo |
15mLCentrifugal tube,50branch/package |
LN0415 |
Cleanert LipoNo has good adsorption effects on monoglycerides, diglycerides, and triglycerides, and has better performance in removing lipid substances than other fillers.
Figure 1. The oil removal performance of four different fillers, Cleanert LipoNo, C18+PSA (mass ratio 1/1), zirconia, and hydrophobic volume exclusion material, with a weight of 1g, was evaluated by observing their removal effects on monoglycerides, diglycerides, and triglycerides, respectively. The comprehensive degreasing effect of Cleanert LipoNo is superior to the other three fillers.
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To investigate the removal efficiency of Cleanert LipoNo and three other materials on chicken tissue matrix, GC/MS full scan was performed on the final extracts before and after purification, and the full scan chromatograms were integrated. The sample matrix removal rate was calculated according to the formula. The results showed that Cleanert LipoNo was more effective in removing matrix interference from chicken samples among the four materials.
Figure 2. After purification with three different materials, the matrix removal efficiency (%) of chicken samples was determined by GC-MS full scan method. The results indicate that Cleanert LipoNo can more effectively remove matrix interference from chicken samples.
After adding the chicken sample, experiments were conducted to eliminate the effects of extraction efficiency and the adsorption of veterinary drugs by the material itself. It is intuitive to see the improvement in recovery rate brought about by the removal of sample matrix effects.
Four materials, Cleanert LipoNo, C18+PSA (mass ratio 1/1), zirconia material, and hydrophobic volume exclusion material, were used to treat chicken samples using the same pre-treatment method. Thirteen sulfonamide veterinary drugs (spiked concentration 20ppb) were added and compared with the standard without a sample matrix to obtain the recovery rates of the 13 sulfonamide drugs. The results showed that Cleanert LipoNo was more effective in reducing matrix effects and had better data stability.
Figure 3. Matrix effect results of sulfonamide drugs. The matrix effect of chicken tissue purified by Cleanert lipoNo was lower than that of samples treated with C18+PSA (mass ratio 1/1), zirconia material, and hydrophobic volume exclusion material
Figure 4. RSD results of sulfonamide drug recovery rate show that the stability of chicken tissue purified by Cleanert lipoNo is better than that of samples treated with C18+PSA (mass ratio 1/1), zirconia material, and hydrophobic volume exclusion material.
Table 1. Recovery rate and RSD results of sulfonamide drugs (n=6)
Drug name |
Average recovery rate (n=6) |
RSD (n=6) |
||||||
Cleanert LipoNo |
C18+PSA |
Zirconia material |
Hydrophobic volume exclusion material |
Cleanert LipoNo |
C18+PSA |
Zirconia material |
Hydrophobic volume exclusion material |
|
Sulfamerazine |
101% |
88% |
98% |
87% |
6% |
15% |
10% |
16% |
Sulfamethazine |
96% |
36% |
43% |
96% |
5% |
17% |
9% |
5% |
Sulfamonomethoxine |
96% |
54% |
64% |
97% |
2% |
20% |
5% |
17% |
Sulfamethizole |
103% |
48% |
56% |
97% |
3% |
8% |
7% |
6% |
Sulfameter |
68% |
102% |
103% |
75% |
3% |
4% |
9% |
20% |
Sulfadimethoxine |
97% |
104% |
106% |
95% |
2% |
2% |
2% |
5% |
Sulfamethoxazole |
109% |
84% |
90% |
97% |
4% |
4% |
4% |
5% |
Sulfisoxazole |
98% |
102% |
106% |
83% |
7% |
2% |
4% |
4% |
Sulfabenzamide |
89% |
103% |
107% |
89% |
3% |
2% |
4% |
5% |
Sulfaquinoxaline |
82% |
96% |
99% |
82% |
4% |
1% |
5% |
6% |
Sulphacetamide |
66% |
69% |
71% |
62% |
3% |
1% |
7% |
19% |
Trimethoprim |
84% |
105% |
110% |
81% |
4% |
6% |
8% |
12% |
Sulfaphenazole |
95% |
95% |
98% |
86% |
3% |
2% |
5% |
7% |
Analysis method for 106 veterinary drug residues in chicken meat
This experiment selected 106 commonly used veterinary drugs, divided into 14 major categories. There are various animal residues, including 1 androgen, 3 sulfonylureas, 32 glucocorticoids, 11 nonsteroides, 18 sulfonamides, 14 nitroimidazoles, 13 quinolones, 4 macrolides, 4 tetracyclines, 1 cephalosporin, 3 chloramphenicol, 1 amantadine, and 1 pyridine.
The sample was extracted with 0.1 mol/L EDTA aqueous solution and acetonitrile, purified with Cleanert LipoNo, detected by LC-MS/MS, separated by Venusil MP C18, and quantified by external standard method. The results showed that the recovery rates of 106 veterinary drugs ranged from 60% to 120%, with RSD less than 20%, which met the detection requirements.
Figure 5. Recovery rates and RSD results of the analysis method for 106 veterinary drug residues in chicken meat. When added at levels of 0.01mg/kg or 0.02mg/kg, the recovery rates of the 106 veterinary drugs ranged from 60% to 120%, with RSD less than 20%, which meets the detection requirements.
Table 2. Experimental results of spiked recovery of 106 animal residues in chicken meat (n=3)
Drug classification |
quantity |
Add level/mg/kg |
Average recovery rate% |
averageRSD% |
Androgens |
1 |
0.01 |
64.6 |
18.0 |
Sulfonylurea class |
3 |
0.01 |
89.4 |
10.7 |
Corticosteroids |
32 |
0.01 |
87.2 |
9.3 |
Non steroidal substances |
11 |
0.01 |
102.6 |
7.2 |
Sulfonamide class |
18 |
0.02 |
78.3 |
4.5 |
Nitroimidazole class |
14 |
0.01 |
98.1 |
7.4 |
Quinolones |
13 |
0.02 |
72.3 |
6.7 |
Macrolides |
4 |
0.02 |
78.0 |
6.6 |
Tetracyclines |
4 |
0.01 |
85.1 |
10.7 |
Cephalosporins |
1 |
0.02 |
71.1 |
2.2 |
Chloramphenicol class |
3 |
0.01 |
103.9 |
13.9 |
Adamantane amine |
1 |
0.01 |
78.0 |
12.3 |
Pyridine class |
1 |
0.01 |
74.7 |
19.5 |
(Please contact Bonaijer Sales for detailed application report)
Rapid detection method for 9 β - receptor agonists in animal derived foods
The commonly used extraction and purification methods for detecting β - receptor agonists are liquid-liquid extraction and solid-phase extraction, which are cumbersome and time-consuming. In this experiment, Cleanert LipoNo was used to purify and remove lipids, and a rapid detection method for 9 β - receptor agonists in three matrices: pig buttocks, cow hind legs, and sheep legs was established. The metabolism of phenol type β - receptor agonists in biological organisms exists in a conjugated state, and their residue detection must go through a hydrolysis process. In the experiment, the sample was homogenized and enzymatically hydrolyzed, then extracted with ammoniated acetonitrile, purified with Cleanert LipoNo, and detected by LC-MS/MS, Kinetex ® F5 is used for separation, and external standard method is used for quantification. The results showed that the recovery rates of enzymatically hydrolyzed pig buttocks, cow hind legs, and sheep legs were all greater than 70%, with RSD less than 20%, meeting the experimental requirements.
Figure 5. Recovery rates and RSD results of 9 rapid detection methods for β - receptor agonists. Adding a level of 5 μ g/Kg, the recovery rates of pig buttocks, cow hind legs, and sheep legs after enzymatic hydrolysis were all greater than 70%, with RSD less than 20%, which can meet the detection requirements.
Table 3. Results of spiked recovery experiments for 9 receptor agonists in muscle tissue (spiked concentration: 5 μ g/Kg)
Pork Butt Meat |
Beef leg meat |
Sheep leg meat |
||||
Average recovery rate,% |
RSD，% |
Average recovery rate,% |
RSD，% |
Average recovery rate,% |
RSD，% |
|
RactopamineRactopamine |
93.8 |
13.9 |
80.0 |
8.1 |
85.3 |
3.2 |
SalbutamolSalbutamol |
85.1 |
0.1 |
74.7 |
8.5 |
74.6 |
0.4 |
TerbutalineTebutalin |
81.8 |
2.4 |
75.5 |
4.8 |
78.0 |
4.7 |
CimaterolXimatero |
91.9 |
8.0 |
85.3 |
3.9 |
88.9 |
3.7 |
ClenbuterolClenbuterol |
85.0 |
12.1 |
89.6 |
4.6 |
80.0 |
2.4 |
TulobuterolTuolotuo |
82.8 |
14.9 |
86.8 |
2.4 |
89.7 |
0.6 |
penbutololSpray Butro |
84.6 |
3.2 |
81.1 |
0.9 |
84.9 |
1.0 |
propanololFeeling at ease |
85.6 |
10.7 |
85.9 |
3.9 |
81.7 |
2.2 |
clorprenalineChlorpheniramine |
90.6 |
13.8 |
96.9 |
4.6 |
89.2 |
7.1 |
(Please contact Bonaijer Sales for detailed application report)