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Sulfonamides are synthetic antibacterial drugs, which are usually used to treat bacterial growth due to their broad-spectrum and hyperspectral activity. Sulfonamides are usually used in the processing of food-grade honey, and their residues are usually present in honey samples, which poses a major risk to consumers around the world. This article describes a case study using the Bruker EVOQ Elite Triple Quadrupole Liquid Chromatography Mass Spectrometer (LC-MS/MS), demonstrating the superior sensitivity and selectivity of the determination of sulfonamides under the required maximum residue limit (MRL). And in accordance with the standards set by the European Commission decision.
Sulfonamide drugs inhibit the production of folic acid by bacteria, thereby preventing the growth and reproduction of bacteria.
Although sulfa drugs are effective against different bacteria, their use is quite limited because they are known to cause extreme allergic reactions in patients with allergies and expose humans to resistant bacteria.
As sulfa exposure poses a potential risk to consumers, different regions have set their own maximum residue limits (MRL), minimum performance levels (MRPL) and specific testing standards to determine sulfa. The European Union has established an MRPL of 10 µg/kg for sulfa drugs in honey. It also sets general standards for the interpretation of test results to ensure the quality and comparability of analytical results produced by approved laboratories for official residue control.
There are a variety of methods that can be used to determine and quantify sulfa drugs in food-grade honey products. However, for complex food matrices, many techniques have poor sensitivity and selectivity, so they cannot be used to determine the content of sulfonamides in honey. For this reason, a combination of liquid chromatography and mass spectrometry can be used to solve this problem.
Figure 1. Sulfonamides are frequently detected in food-grade honey.
A case study showed how to use EVOQ Elite LC-MS/MS to detect a sulfonamide level of 0.1 ppb with a constant ion ratio of quantifier to qualifier ion. This method can quickly and simply quantify sulfa drugs in honey, and the results show that it is repeatable and linear, with relative standard deviation (RSD) <12%, regression (R) = 0.996. EVOQ has high specificity and sensitivity, and is flexible enough to achieve high sample throughput for the detection and quantification of sulfa drugs.
The high sensitivity of EVOQ reflects a number of hardware innovations in the ion source, such as Active Exhaust that suppresses the recirculation of atomized gas, thereby reducing chemical noise. This also means less downtime and eliminates the time to clean and run samples, thereby providing high productivity and excellent sensitivity in high-throughput laboratories.
In addition, Bruker's PACER software complements EVOQ's hardware, which provides anomaly-based data review to significantly reduce the error rate of quantitative analysis. In this way, PACER improves efficiency by reducing the scanning time that affects data quality, and speeds up the time from sample to report, which is very important for laboratories engaged in routine quantitative work.
Use EVOQ Elite triple quadrupole liquid chromatography mass spectrometer to determine nine sulfonamides in honey, as shown in the following table:
Table 1. EVOQ tested nine commonly used sulfa drugs.
For sample preparation, prepare a standard mixed solution of all nine sulfonamides at a concentration of 1000 ng/mL by diluting the individual sulfonamide stock solutions with triple distilled water and acetonitrile. Then, prepare the calibration solution by adding an appropriate volume of the mixed standard solution to the blank honey matrix. The instrument calibration used is as follows:
Figure 2. Chromatograms of all nine sulfonamides in honey analyzed at a LOQ concentration of 0.1ppb, with peak-to-peak signal-to-noise ratio.
Figure 3. Overlaid chromatograms of all nine sulfa drugs and a blank honey matrix at the LOQ level.
Figure 2 shows the chromatograms of all nine sulfonamides detected in honey at a concentration of 0.1 ppb, with peak-to-peak signal-to-noise ratio (S/N). It was found that the S/N ratio of all nine sulfonamides in the honey matrix was 0.1 ppb, which was much higher than 10. Figure 3 clearly shows that the blank honey matrix does not contain any target sulfonamides.
This case study was conducted in accordance with European Union Decision 2002/657/EC, which specifies many parameters to confirm the detection of target compounds.
This technique is repeatable, with RSD less than 12%, as shown in Table 2. The results obtained for all nine sulfa drugs at the limit of quantification of 0.1 ng/g are within a satisfactory accuracy range. In addition, the limit of quantification of all nine sulfonamides studied is 0.1 ng/g, which is much lower than the MRL required by laws and regulations in different regions.
Table 2. Summary of the properties of sulfa drugs in honey.
Bruker's EVOQ Elite Liquid Chromatography Mass Spectrometer provides excellent repeatability and detection limits for all nine sulfonamides studied in the honey matrix. This, combined with PACER software, can provide consistent results in the fastest time. The use of Advance UHPLC also significantly reduces the total chromatographic run time. Therefore, the combination of faster sample-to-report time, higher sensitivity, and low maintenance make EVOQ suitable for processing complex samples in high-throughput laboratories.
This information is derived from materials provided by Bruker-Chemistry and Applied Markets, which has been reviewed and adapted.
For more information on this source, please visit Bruker Daltonics.
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Brooke Dalton Studies. (March 4, 2021). A triple quadrupole liquid chromatography mass spectrometer was used to detect sulfonamides in food-grade honey. AZoM. Retrieved from https://www.azom.com/article.aspx?ArticleID=10657 on December 14, 2021.
Brooke Dalton Studies. "Using a triple quadrupole liquid chromatography mass spectrometer to detect sulfonamides in food-grade honey". AZoM. December 14, 2021. <https://www.azom.com/article.aspx?ArticleID=10657>.
Brooke Dalton Studies. "Using a triple quadrupole liquid chromatography mass spectrometer to detect sulfonamides in food-grade honey." AZoM. https://www.azom.com/article.aspx?ArticleID=10657. (Accessed on December 14, 2021).
Brooke Dalton Studies. 2021. Use a triple quadrupole liquid chromatography mass spectrometer to detect sulfonamides in food-grade honey. AZoM, viewed on December 14, 2021, https://www.azom.com/article.aspx?ArticleID=10657.
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