LC-MS/MS Method, Development and Validation to Determine Three Tetracyclines and Their Epimers in Shrimp Samples

REDDY, B. SIDDA; Sudhakar, Y.; Rao, Yifei; Reddyprasad, P.; Sreedhar, N. Y.

doi:10.13005/ojc/330539

Cited by 7 publications

(7 citation statements)

References 16 publications

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“…Thus, control of tetracyclines and their 4-epimers has attracted interest in many studies, which mainly focused on the quantitative determination by liquid chromatography (LC)/MS. [9][10][11][12][13][14] Only two studies investigated the differentiation of tetracyclines by MS fragment ions. 15,16 So, a pair of tetracycline-like diastereomers could be differentiated.…”

Section: Discussionmentioning

confidence: 99%

Diastereomer recognition of three pairs of tetracyclines by electrospray ionization mass spectrometry

Zhu

Zhou

Jiang

et al. 2021

Rapid Comm Mass Spectrometry

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Rationale Stereoisomer profiling is always a difficult issue. Based on the difference between diastereomers, usually because of steric hindrance, isomers can be differentiated by mass spectrometry (MS), although it is often not an easy task. In the current study, tetracycline, chlortetracycline and doxycycline could be distinguished from their respective 4‐epimers by MS. Methods The electrospray ionization tandem mass spectrometry (ESI‐MSn) analyses were carried out on a Bruker 3000plus ion trap mass spectrometer. For MS/MS experiments, the collision energy was set between 0.18 and 0.45 V to perform energy‐resolved mass spectrometry (ERMS). Test solutions were prepared in methanol/water (90:10, v/v) at a concentration of 10 μg/mL. Results Compared with the collision‐induced dissociation (CID) spectrum of protonated tetracycline, the most abundant peak changed from m/z 427 to m/z 410 for 4‐epitetracycline. For chlortetracycline and its 4‐epimer, differences in relative abundance were observed too. In the CID spectrum of a fragment ion of doxycycline, the abundance of m/z 154 was relatively higher than for the 4‐epimer, showing the same trend as in the CID spectra of the other two pairs of tetracyclines. Conclusions The CID spectra of tetracycline and chlortetracycline were different from those of their 4‐epimers. The CID spectra of protonated doxycycline and its 4‐epimer showed only a subtle difference, but the m/z 154 fragment ion in the CID spectra of the fragment ion at m/z 428 offers the possibility to differentiate both epimers.

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Section: Discussionmentioning

confidence: 99%

Diastereomer recognition of three pairs of tetracyclines by electrospray ionization mass spectrometry

Zhu

Zhou

Jiang

et al. 2021

Rapid Comm Mass Spectrometry

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“…The linearity was evaluated by constructing a matrix‐matched calibration curve using six concentrations ranging from 5 to 50 μg/kg, and the plot of the curve for each compound was based on the peak areas of analyte at various concentrations. The LODs and LOQs were calculated according to the standard deviation (STEYX) of the mean response and the slope of the linear plot (Reddy, Sudhakar, Rao, Reddyprasad, & Sreedhar, ). The accuracy and precision were estimated by analysing blank duck meat samples spiked at three concentrations: 5, 10, and 20 μg/kg.…”

Section: Methodsmentioning

confidence: 99%

Development and validation of a solid‐phase extraction method coupled with LC–MS/MS for the simultaneous determination of 16 antibiotic residues in duck meat

Zheng

El‐Aty

Kim

et al. 2019

Biomedical Chromatography

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The present study was carried out to determine 16 antibiotics belonging to seven different groups (tetracyclines, sulfonamides, penicillins, fluoroquinolones, macrolides, lincosamides and trimethoprims) in duck meat. A solid‐phase extraction method based on Oasis HLB cartridges coupled with liquid chromatography–electrospray ionization tandem mass spectrometry was developed. Solutions of 0.1 m ethylenediaminetetraacetic acid disodium salt and 2% trifluoroacetic acid were used for the preliminary extraction of the target antibiotics from duck meat and n‐hexane was used for purification prior to solid‐phase extraction. Mobile phases composed of 0.1% trifluoroacetic acid in distilled water (solvent A) and 0.1% trifluoroacetic acid in methanol (solvent B), combined with a reversed‐phase C18 analytical column, provided the optimal separation and signal intensity. The linearity of the method was assessed using six concentrations (5, 10, 20, 30, 40, and 50 μg/kg), and the recoveries, which were calculated at three spiking concentrations (5, 10 and 20 μg/kg), were in the range 69.8–103.3% with relative standard deviations (RSDs) ≤ 6.9% for the 16 tested antibiotics. Matrix effects ranging from −47.2 to −13.5% were observed for all the analytes, and the limits of quantitation (LOQ), which ranged from 4.93 to 26.21 μg/kg, were much lower than the maximum residue limits (MRLs) set by various regulatory authorities. Ten samples from a market were tested, and none of the target analytes were detected. Thus, a simple and versatile protocol has been developed to detect and quantify 16 antibiotics in duck meat samples.

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“…In addition, an economic saving was also achieved by decreasing the run time to just 10 min, The LOQ 38.22, 33.20, 26.22, and 11.32 µg/kg, respectively, Tet + , Oxy-tet + , Chlor-tet + , and doxycycline [31]. [32]. Ribeiro et al [33] developed and validated a method to determine Sulfa + , Tet + , and macrolides in honey sample, using LC-MS/MS according to Council Directive 657/EC/2002.…”

Section: Lc-msmentioning

confidence: 99%

“…Linearity coefficient of determination was (R2) <0.99, LOD 17.93, 16.04, 19.67, 20.54, 20.52, and 18.98 for 4-epi-chlortet + , 4-epi Oxy-tet + , Chlor-tet + , 4-epi-tet + , Oxy-tet + , Tet + , respectively, and LOQ was 54.35, 48.63, 59.62, 62.26, 62.18, and 57.54 for 4-epi Chlor-tet + , Epi-Oxy-tet + , 4-epi-tet + , Chlor-tet + , Oxy-tet + , and Tet + , respectively. Recovery ranged measured between 83.07 and 115.58%, DL measured between 108.24 and 114.48 and DC was 116.48-129.61 [ 32 ]. Ribeiro et al .…”

Section: Lc-msmentioning

confidence: 99%

Assessment of various veterinary drug residues in animal originated food products

Parmar

Chaubey

Gupta³

et al. 2021

Vet World

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The veterinary drugs are broad-spectrum antibacterial antibiotics; it uses to cure the animal disease. Many countries have banned veterinary drug residues like nitrofurans metabolites, chloramphenicol. However, the people were administrated veterinary drugs to animals as illegal to increase the milk production in animals for economic benefit. The results of illegally use of veterinary drugs remain as a residue in animal product like milk and it is very harmful to whom consume it cause cancer and allergic for human being which has entered the concern among milk consumers. To control illegal use of veterinary drugs, the government of India has restricted its use in animals. For the identification and confirmation of veterinary drug residues in animal products, analytical techniques such as liquid chromatography and mass spectrometry are available. These are very sophisticated equipments which are available nowadays and their methodologies for the analytical method validation are described by European commission 2002/657/EC. The use of veterinary drugs is a big challenge to effectively identify and authorization of their use. There are so many analytical techniques are using very effectively and taking very less time to protect the consumers from their adverse effects. These techniques take very less time to identify more groups of compounds such as tetracycline, sulfonamides, anthelmintic, and macrolides in single multi-residue method. These methods having validation parameters include system precision, calibration curve, accuracy, limit of detection, and quantification. Therefore, improvement in the existing technologies and accessibility of new screening methodologies will give opportunities for automation that helps in obtaining the results in very less time and improved sensitivity and specificity which contribute to better safety assurance, standard, and quality of various food products of animal origin.

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LC-MS/MS Method, Development and Validation to Determine Three Tetracyclines and Their Epimers in Shrimp Samples

Cited by 7 publications

References 16 publications

Diastereomer recognition of three pairs of tetracyclines by electrospray ionization mass spectrometry

Diastereomer recognition of three pairs of tetracyclines by electrospray ionization mass spectrometry

Development and validation of a solid‐phase extraction method coupled with LC–MS/MS for the simultaneous determination of 16 antibiotic residues in duck meat

Assessment of various veterinary drug residues in animal originated food products

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