Multi-residue screening of veterinary drugs in egg, fish and meat using high-resolution liquid chromatography accurate mass time-of-flight mass spectrometry

Peters, Ruud; Bolck, Y.J.C.; Rutgers, Paula; Stolker, A.A.M.; Nielen, Michel W. F.

doi:10.1016/j.chroma.2009.04.027

Cited by 183 publications

(94 citation statements)

References 26 publications

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“…However, in the last few years, there have been an increased number of publications on multi-class methods for analysis of veterinary drugs in food using either LC-MS/MS or LC-TOF instruments. The extraction techniques that have been reported included a molecular weight cut-off filter (3 kD) for milk (150 veterinary drugs), [8] liquid-liquid extraction (LLE) for honey (42 antibiotics), [9] solid-phase extraction (SPE) using StrataX for egg, milk, animal tissues (100 veterinary drugs), [10,11] and QuEChERS for animal tissues (41 veterinary drugs), [12] and milk (21 veterinary drugs) [13] for different classes of veterinary drugs at various concentrations.…”

Section: Introductionmentioning

confidence: 99%

The challenges of developing a generic extraction procedure to analyze multi‐class veterinary drug residues in milk and honey using ultra‐high pressure liquid chromatography quadrupole time‐of‐flight mass spectrometry

Wang

Leung

2012

Drug Testing and Analysis

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This paper discusses the analytical challenges to develop a generic extraction procedure to analyze or screen multi-class veterinary drugs in milk and honey using ultra-high pressure liquid chromatography quadrupole time-of-flight mass spectrometry (UHPLC QqTOF MS). The veterinary drugs in this study included aminoglycosides, endectocides, fluoroquinolones, ionophores, b-lactams or penicillins, macrolides, NSAIDs, phenicols, sulfonamides and tetracyclines. Veterinary drugs were extracted using a QuEChERS (quick, easy, cheap, effective, rugged, and safe) method, which entailed the use of acetonitrile containing 1% acetic acid, sodium acetate, ethylenediaminetetra acetic acid disodium (EDTA) and magnesium sulfate, and no clean-up was performed. Chromatographic separation was achieved on a reversed-phase Acquity UPLC BEH C 18 , 100 Â 2.1 mm, 1.7 mm column with 0.1% formic acid and 10 mM ammonium formate in water, and acetonitrile as mobile phases. Due to poor chromatographic retention, aminoglycosides were first dropped from the list, and because of poor extractability, b-lactams and tetracyclines were also excluded from the method. The method was able to quantify 31 or screen up to 54 drugs (unbound) in honey, and to quantify 34 or screen up to 59 drugs in milk. UHPLC QqTOF data were acquired in TOF MS full-scan mode that allowed both quantification and confirmation of veterinary drugs and identification of their degradation products in samples. The method could achieve detection limits as low as 1 mg/kg with analytical range from 1 to 100 mg/kg. The developed method was intended to be used for screening of as many analytes as possible in one single analysis, or unequivocal confirmation of positive findings and degradation product identification based on accurate mass measurement and isotopic patterns.

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Section: Introductionmentioning

confidence: 99%

The challenges of developing a generic extraction procedure to analyze multi‐class veterinary drug residues in milk and honey using ultra‐high pressure liquid chromatography quadrupole time‐of‐flight mass spectrometry

Wang

Leung

2012

Drug Testing and Analysis

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“…In this case, the delta value was 0.0118, and the mass error was 2 mDa. Similarly, the identification of the steroid hormones was performed using the SigmaFit algorithm, and the identified steroids were then quantified by LC-MS/MS analysis (22). Other steroids were identified by same procedure as shown in Supplementary Fig.…”

Section: Steroidsmentioning

confidence: 99%

Accurate determination of tissue steroid hormones, precursors and conjugates in adult male rat

Maeda

Tanaka

Suzuki

et al. 2012

The Journal of Biochemistry

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The actual levels of steroid hormones in organs are vital for endocrine, reproductive and neuronal health and disorders. We developed an accurate method to determine the levels of steroid hormones and steroid conjugates in various organs by an efficient preparation using a solid-phase-extraction cartridge. Each steroid was identified by the precursor ion spectra using liquid chromatographyelectrospray ionization timeof-flight mass spectrometry, and the respective steroids were quantitatively analysed in the selected reaction monitoring mode by liquid chromatograph-mass spectrometry/mass spectrometry (LC-MS/MS). The data showed that significant levels of testosterone, corticosterone and precursors of both hormones were detected in all organs except liver. The glucuronide conjugates of steroid hormones and the precursors were detected in all organs except liver, but sulfate conjugates of these steroids were observed only in the target organs of the hormones and kidney. Interestingly, these steroids and the conjugates were not observed in the liver except pregnenolone. In conclusion, an accurate determination of tissue steroids was developed using LC-MS analysis. Biosynthesis of steroid hormones from the precursors was estimated even in the target organs, and the delivery of these steroid conjugates was also suggested via the circulation without any significant hepatic participation.

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“…[11,12] In this example, the focus is on the validation of tetracycline, oxytetracyline, and sulfamethoxazole in meat and eggs. Table 1 shows the MRLs for the registered drugs for meat and eggs.…”

Section: Full-scan Ms Analysis Of Antibioticsmentioning

confidence: 99%

Application of EU guidelines for the validation of screening methods for veterinary drugs

Stolker

2012

Drug Testing and Analysis

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Commission Decision (CD) 2002/657/EC describes detailed rules for method validation within the framework of residue monitoring programmes. The approach described in this CD is based on criteria. For (qualitative) screening methods, the most important criteria is that the CCb has to be below any regulatory limit. Especially when microbiological or immunochemical methods are involved, the approach described in the CD is not easily applied. For example, by those methods, a large number of analytes (all antibiotics) within several different matrices (meat, milk, fish, eggs, etc.) are detected. It is not completely clear whether all those analytes and all matrices have to be taken into account during method validation. To clarify this, a working group -from EU Reference Laboratories -came up with a practical approach to validate multi-analyte multi-matrix screening methods. It describes how many analyte/matrix combinations have to be tested and how these combinations are selected. Furthermore it describes how to determine CCb for screening methods in relation to a large list of compounds and maximum residue limits (MRLs). First for each analyte/matrix combination the 'cut-off' level -i.e. the level at which the method separates blanks from contaminated samples -is established. The validation is preferably at the concentration of 50% of the regulatory limit. A minimum set of 20 different samples has to be tested. From the experiences with applying these guidelines it was concluded that the validation approach is very 'practical'; however, there are some remarks. One has to be careful with selecting 'representative' analytes and matrices and it is strongly recommended to collect additional validation data during the routine application of the method.

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Multi-residue screening of veterinary drugs in egg, fish and meat using high-resolution liquid chromatography accurate mass time-of-flight mass spectrometry

Cited by 183 publications

References 26 publications

The challenges of developing a generic extraction procedure to analyze multi‐class veterinary drug residues in milk and honey using ultra‐high pressure liquid chromatography quadrupole time‐of‐flight mass spectrometry

The challenges of developing a generic extraction procedure to analyze multi‐class veterinary drug residues in milk and honey using ultra‐high pressure liquid chromatography quadrupole time‐of‐flight mass spectrometry

Accurate determination of tissue steroid hormones, precursors and conjugates in adult male rat

Application of EU guidelines for the validation of screening methods for veterinary drugs

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