Determination of sulfonamides in beeswax by liquid chromatography coupled to tandem mass spectrometry

Mitrowska, Kamila; Antczak, Maja

doi:10.1016/j.jchromb.2015.10.040

Cited by 13 publications

(10 citation statements)

References 13 publications

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“…It should be noted that the existing methods of control -organoleptic, chemical, physical, -although reliable, but morally and technically obsolete [11,12], and do not correspond to the current level of quality control of products of beekeeping [13,14]. An urgent need for modern methods of quality control [15,16] is due to the fact that fake beeswax is a direct threat to the existence of honey bees, and can negatively affect the quality of all products of beekeeping.…”

Section: Introductionmentioning

confidence: 99%

Identification of beeswax and its falsification by the method of infrared spectroscopy

Vyshniak¹,

Dimitriev²,

Litvynchuk³

et al. 2018

Ukr. food j.

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Introduction. The purpose of the research was to determine the characteristics of the infrared spectra of reflection and absorption of beeswax, as well as wax with the content of impurities in it, in particular paraffin and ceresin. Materials and methods. Natural beeswax, paraffin, ceresin, as well as their mixtures were investigated by infrared spectroscopy of reflection and absorption using Infrapid-61, Luminar 5030 and SPECORD M-80 spectrometers. Results and discussion. Infrared reflection spectra from smooth surfaces of samples (paraffin, ceresin, wax, a mixture of beeswax and ceresin, a mixture of wax paraffin and ceresin, a mixture of wax and paraffin) have a similar structure. There are two clearly expressed maxima at wavelengths of 1510 and 1581 nm. The ratio R w (1581)/R w (1510) varies from 1.115 to 1.265. The smallest value corresponds to natural beeswax, and the maximum value is ceresin. After shredding the sample, the infrared spectral diffuse reflections did not undergo significant changes, the most intense spectral maxima did not change its position, but the redistribution of spectral lines by intensity was happened out. There were pronounced differences in the region from 1723 to 2400 nm. The coefficient  for the reflection spectra from the smooth surface was ~ 1.2, and for the reflection spectra from the crushed samples ~ 1.1. The reflection spectra in the region from 1100 to 1350 nm have a clear maximum at a wavelength of 1212.5 nm. IR reflection spectra allowed us to clarify the difference between the natural beeswax and ceresin through the ratio of reflection features at 1510 and 1581 nm: the maximal ratio corresponded to the former, while the smallest one to the latter. The different proportion of bands corresponding to CH 2 and CH 3 stretching vibrations suggested that hydrocarbon chains of wax molecules are longer than those of paraffin and ceresin studied. It was found that hydrocarbon contaminants in the bee wax are associated with narrowing of the C=O band at ~1736 cm-1. Conclusions. The detected spectral laws will enable the identification of natural beeswax and detect its counterfeit.

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Section: Introductionmentioning

confidence: 99%

Identification of beeswax and its falsification by the method of infrared spectroscopy

Vyshniak¹,

Dimitriev²,

Litvynchuk³

et al. 2018

Ukr. food j.

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“…Many HPLC columns used in previous studies have shown excellent efficiency in the sufficient baseline separation of SAs; however, analysis time using these columns for 12–24 SAs is 20–30 min at a run, − and the major drawback is the high cost of organic solvents. For shorter analysis time, some UPLC columns have been applied to the separation of 14–20 SAs − only. Therefore, the simultaneous and complete separation of 27 SAs is an interesting challenge.…”

Section: Resultsmentioning

confidence: 99%

“…Many different extractants have been suggested for extracting SAs in different materials, including AC, acid solution, and mixtures of AC and water. − ,− However, few studies focused on the extraction of SAs in poultry feathers. , Because the accumulation of organic drugs in hair was first described in the 1950s, the four main procedures used to extract analytes from the hair samples include acid, base, enzyme, and mixed–organic solvent extraction . The solution extraction efficiency was evaluated using positive feather samples containing one typical SA SMZ and blank feather samples spiked with 100 ng/g of SAs.…”

Section: Resultsmentioning

confidence: 99%

“…Current detection methods for SAs residues include immunoassays, liquid chromatography, and liquid chromatography–tandem mass spectrometry (LC–MS/MS). − ,− LC–MS/MS is the most useful confirmatory analysis technique because of its high sensitivity. LC–MS/MS methods have been successfully used to determine 14–24 SAs in various matrices, including animal tissue, honey, milk, runoff water, and soils.…”

Section: Introductionmentioning

confidence: 99%

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Multiresidue Determination of 27 Sulfonamides in Poultry Feathers and Its Application to a Sulfamethazine Pharmacokinetics Study on Laying Hen Feathers and Sulfonamide Residue Monitoring on Poultry Feathers

Suo

Wang

Xiao

et al. 2019

J. Agric. Food Chem.

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A method for the simultaneous determination of 27 sulfonamides in poultry feathers using ultra performance liquid chromatography−tandem mass spectrometry (UPLC−MS/MS) was established in this study. The samples were extracted using 0.1 mol/L HCl solutions in a 60 °C water bath for 2 h, purified using hydrophilic−lipophilic balance solid-phase extraction, nitrogen-dried, and then reconstituted for UPLC−MS/MS analysis, which was performed with a CSH-C18 column. Linearity, limit of detection, limit of quantification, recovery, and precision were calculated in accordance with Commission Decision 2002/657/EC. For linearity, all standard curves showed a standard coefficient greater than 0.99, and the recoveries and coefficient of variation were 89−115% and <20%, respectively. The limit of detection and limit of quantification were 0.2−5 and 0.5−20 ng/g, respectively. The method was successfully applied to sulfamethazine (SMZ) residue accumulation monitoring in laying hen feathers and sulfonamide residue monitoring on poultry feathers. SMZ residue accumulation in the laying hen feathers was studied after administration with 100 mg/kg of SMZ for 21 consecutive days. SMZ residues were still detected in feathers 14 days after drug administration and persisted for up to 85 days. Results from 42 poultry feather samples showed that the feather is a suitable medium to monitor the illegal use of sulfonamides in poultry production.

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“…Therefore, the residues of antibiotics are a significant risk for the quality of bee products and for human health. The accumulation of antibiotics like sulfonamides in beeswax has been well documented . But no information about tetracycline residues in beeswax has been reported and no reference for determination of TCs in beeswax has been found.…”

Section: Introductionmentioning

confidence: 99%

Development, validation and application to real samples of a liquid chromatography with tandem mass spectrometry method for the determination of tetracyclines in beeswax

Gajda

Antczak

Mitrowska

et al. 2018

J of Separation Science

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Beeswax is a valuable honeybee product, which finds applications in the food and pharmaceutical industries, as well as in cosmetic production. However, some substances used in apiculture, like tetracyclines, can be delivered to hives where they cause contamination of honeybee products such as beeswax. Tetracyclines are commonly used for the treatment of American and European foulbrood diseases, but in the European Union their usage by beekeepers is forbidden. Thus, a sensitive method for the analysis of tetracyclines in beeswax is an important analytical tool. A new liquid chromatography with tandem mass spectrometry method for the analysis of tetracyclines including oxytetracycline, 4-epioxytetracycline, tetracycline, 4-epitetracycline, chlorotetracycline, 4-epichlorotetracycline, and doxycycline in beeswax was developed. The method involved dilution of beeswax in n-hexane after a melting step, liquid-liquid extraction with oxalic acid and clean-up using a weak cation exchange phase. Satisfactory separation was performed on an octadecyl column with 0.1% formic acid and acetonitrile in a total run time of 5 min. The application of this method was evaluated by the analysis of real beeswax samples. The presence of oxytetracycline was confirmed in 5 out of 48 tested beeswax samples, which shows the method can be successfully used to determine the tetracyclines in beeswax.

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Determination of sulfonamides in beeswax by liquid chromatography coupled to tandem mass spectrometry

Cited by 13 publications

References 13 publications

Identification of beeswax and its falsification by the method of infrared spectroscopy

Identification of beeswax and its falsification by the method of infrared spectroscopy

Multiresidue Determination of 27 Sulfonamides in Poultry Feathers and Its Application to a Sulfamethazine Pharmacokinetics Study on Laying Hen Feathers and Sulfonamide Residue Monitoring on Poultry Feathers

Development, validation and application to real samples of a liquid chromatography with tandem mass spectrometry method for the determination of tetracyclines in beeswax

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