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Determination of Histamine in Silages Using Nanomaghemite Core ( γ -Fe 2 O 3 )-Titanium Dioxide Shell Nanoparticles Off-Line Coupled with Ion Exchange Chromatography

View Article: PubMed Central - PubMed

ABSTRACT

The presence of biogenic amines is a hallmark of degraded food and its products. Herein, we focused on the utilization of magnetic nanoparticles off-line coupled with ion exchange chromatography with post-column ninhydrin derivatization and Vis detection for histamine (Him) separation and detection. Primarily, we described the synthesis of magnetic nanoparticles with nanomaghemite core (γ-Fe2O3) functionalized with titanium dioxide and, then, applied these particles to specific isolation of Him. To obtain further insight into interactions between paramagnetic particles’ (PMP) surface and Him, a scanning electron microscope was employed. It was shown that binding of histamine causes an increase of relative current response of deprotonated PMPs, which confirmed formation of Him-PMPs clusters. The recovery of the isolation showed that titanium dioxide-based particles were able to bind and preconcentrate Him with recovery exceeding 90%. Finally, we successfully carried out the analyses of real samples obtained from silage. We can conclude that our modified particles are suitable for Him isolation, and thus may serve as the first isolation step of Him from biological samples, as it is demonstrated on alfalfa seed variety Tereza silage.

No MeSH data available.


Related in: MedlinePlus

(A) Typical IE chromatogram of standard solution composed of selected BAs (100 µg·mL−1); (B) Calibration curves measured under the optimal conditions are shown for Histamine, Cadaverine, Tyramine, Spermindine, Spermine, and Putrescine.
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ijerph-13-00904-f002: (A) Typical IE chromatogram of standard solution composed of selected BAs (100 µg·mL−1); (B) Calibration curves measured under the optimal conditions are shown for Histamine, Cadaverine, Tyramine, Spermindine, Spermine, and Putrescine.

Mentions: Determination of Him in the silage of other plant samples is not an easy task regarding the demands of sensitivity and precision of measurements and the influences of the matrix on the sample pre-treatment steps. The conditions for BA separation and detection using IEC with ninhydrin post-column derivatization and dual channel Vis detection (λ = 570 nm, and 440 nm) were optimized in our preliminary study [15]. In this study, we attempted to combine previously found advantages of PMP-based isolation of the BAs. Based on the optimization of separation of biogenic amines, the conditions were as follows: elution of biogenic amines was performed using gradient elution with buffers of different ionic strength and pH, as well as a temperature gradient. Finally, for detection of His, the elution buffer was used (composition is mentioned in the Materials and Methods—ion-exchange chromatography section), and His was eluted under the following program: 0–45 min elution with buffer A. After separation, the column was regenerated using 0.2 mol·L−1 NaOH for 15 min, and stabilized for 19 min using buffer A. The column temperature was set to 76 °C. Standards of BAs, particulalry Him, Spd, Cad, Put, Spm, and Tym (100 µg·mL−1), measured under the optimal conditions are shown in Figure 2A. Calibration curves of BAs measured under the optimal conditions are shown in Figure 2B. Correlation coefficient equal to 0.9978 was obtained for peak area based calibration curve for determination of Him, indicating strictly linear dependencies. These values were comparable with other reported UV and fluorescence detection levels obtained using various derivatization agents [26,27].


Determination of Histamine in Silages Using Nanomaghemite Core ( γ -Fe 2 O 3 )-Titanium Dioxide Shell Nanoparticles Off-Line Coupled with Ion Exchange Chromatography
(A) Typical IE chromatogram of standard solution composed of selected BAs (100 µg·mL−1); (B) Calibration curves measured under the optimal conditions are shown for Histamine, Cadaverine, Tyramine, Spermindine, Spermine, and Putrescine.
© Copyright Policy
Related In: Results  -  Collection

License
Show All Figures
getmorefigures.php?uid=PMC5036737&req=5

ijerph-13-00904-f002: (A) Typical IE chromatogram of standard solution composed of selected BAs (100 µg·mL−1); (B) Calibration curves measured under the optimal conditions are shown for Histamine, Cadaverine, Tyramine, Spermindine, Spermine, and Putrescine.
Mentions: Determination of Him in the silage of other plant samples is not an easy task regarding the demands of sensitivity and precision of measurements and the influences of the matrix on the sample pre-treatment steps. The conditions for BA separation and detection using IEC with ninhydrin post-column derivatization and dual channel Vis detection (λ = 570 nm, and 440 nm) were optimized in our preliminary study [15]. In this study, we attempted to combine previously found advantages of PMP-based isolation of the BAs. Based on the optimization of separation of biogenic amines, the conditions were as follows: elution of biogenic amines was performed using gradient elution with buffers of different ionic strength and pH, as well as a temperature gradient. Finally, for detection of His, the elution buffer was used (composition is mentioned in the Materials and Methods—ion-exchange chromatography section), and His was eluted under the following program: 0–45 min elution with buffer A. After separation, the column was regenerated using 0.2 mol·L−1 NaOH for 15 min, and stabilized for 19 min using buffer A. The column temperature was set to 76 °C. Standards of BAs, particulalry Him, Spd, Cad, Put, Spm, and Tym (100 µg·mL−1), measured under the optimal conditions are shown in Figure 2A. Calibration curves of BAs measured under the optimal conditions are shown in Figure 2B. Correlation coefficient equal to 0.9978 was obtained for peak area based calibration curve for determination of Him, indicating strictly linear dependencies. These values were comparable with other reported UV and fluorescence detection levels obtained using various derivatization agents [26,27].

View Article: PubMed Central - PubMed

ABSTRACT

The presence of biogenic amines is a hallmark of degraded food and its products. Herein, we focused on the utilization of magnetic nanoparticles off-line coupled with ion exchange chromatography with post-column ninhydrin derivatization and Vis detection for histamine (Him) separation and detection. Primarily, we described the synthesis of magnetic nanoparticles with nanomaghemite core (γ-Fe2O3) functionalized with titanium dioxide and, then, applied these particles to specific isolation of Him. To obtain further insight into interactions between paramagnetic particles’ (PMP) surface and Him, a scanning electron microscope was employed. It was shown that binding of histamine causes an increase of relative current response of deprotonated PMPs, which confirmed formation of Him-PMPs clusters. The recovery of the isolation showed that titanium dioxide-based particles were able to bind and preconcentrate Him with recovery exceeding 90%. Finally, we successfully carried out the analyses of real samples obtained from silage. We can conclude that our modified particles are suitable for Him isolation, and thus may serve as the first isolation step of Him from biological samples, as it is demonstrated on alfalfa seed variety Tereza silage.

No MeSH data available.


Related in: MedlinePlus