Determination of eight penicillins in serum from cattle and pigs by generic HPLC method

Sørensen, Lambert K.; Snor, Lena

doi:10.1007/bf02491068

Cited by 10 publications

(4 citation statements)

References 26 publications

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“…Several analytical methods have been reported in the literature for the determination of Nafcillin and/or its related substances [ 11 – 13 ]. The USP has also published the monographs for both active pharmaceutical ingredients and formulation products and has given the methodologies for determining the assay of Nafcillin [ 14 ].…”

Section: Introductionmentioning

confidence: 99%

Identification, Isolation, and Characterization of a New Degradation Impurity in Nafcillin Sodium

et al. 2015

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A new degradant of Nafcillin Sodium was found at a level of 1.8% w/w during the gradient reversed-phase HPLC analysis in stability storage samples. This impurity was identified by LC-MS and was characterized by 1H-NMR, 13C-NMR, LC/MS/MS, elemental analysis, and IR techniques. Based on the structural elucidation data, this impurity was named as N-[(2S)-2-carboxy-2-{[(2-ethoxynaphthalen-1-yl)carbonyl]amino}ethylidene]-3-({N-[(2-ethoxynaphthalen-1-yl)carbonyl]glycyl}sulfanyl)-D-valine. This impurity was prepared by isolation and was co-injected into the HPLC system to confirm the retention time. To the best of our knowledge, this impurity has not been reported elsewhere. The identification and structural elucidation of this degradant impurity has been discussed in detail.

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Section: Introductionmentioning

confidence: 99%

Identification, Isolation, and Characterization of a New Degradation Impurity in Nafcillin Sodium

et al. 2015

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“…In the majority of papers, HPLC methods utilize UV detection at low wavelengths (f 230 nm) [9,10], although fluorimetric [8] and mass spectrometric detection [7] have also been reported. Sample preparation methods involve deproteinization and extraction techniques, such as LLE or for the most part SPE [1,5,6,13].…”

Section: Introductionmentioning

confidence: 99%

“…The method was linear in the range tested up to 2 ng/lL of individual penicillins in serum. LODs were 11 -14 ng/mL [13].…”

Section: Introductionmentioning

confidence: 99%

Development and validation of an HPLC method for the determination of seven penicillin antibiotics in veterinary drugs and bovine blood plasma

Samanidou¹,

Giannakis

Papadaki

2009

J of Separation Science

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Development and validation of an HPLC method for the determination of seven penicillin antibiotics in veterinary drugs and bovine blood plasma Herein a quantitative method for the determination of seven penicillins in bovine plasma and veterinary drugs has been developed. Amoxicillin (AMO), ampicillin (AMP), penicillin G (PENG), penicillin V (PENV), oxacillin (OXA), cloxacillin (CLO) and dicloxacillin (DICLO) were separated on a Perfectsil ODS-2 (25064 mm, 5 lm) column, using gradient elution, with a mobile phase of 0.1% v/v TFA and ACN -methanol (90:10 v/v). PDA detection was used at 240 nm. Penicillins were isolated from bovine plasma by SPE on Lichrolut RP-18 cartridges with mean recoveries from 85.7 to 113.5%. Colchicine (3 ng/lL) was used as an internal standard. The developed method was validated in terms of selectivity, linearity, accuracy, precision, stability and sensitivity. Repeatability (n = 5) and between-day precision (n = 5) revealed RSD a 12%. The detection limits in the bovine plasma were estimated as 18 ng for AMO and AMP, 25 for PENG, PENV and OXA, 3 ng for CLO and 12 ng for DICLO. Spiked plasma samples were stable for 1 wk, except for AMP and CLO, which were stable for 3 wk and OXA for 4 wk. AMO, PENG and PENV were stable for two freeze -thaw cycles, OXA, CLO and DICLO for four, while AMP only for one.

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“…Further cleanup is achieved by column switching [6] and extraction techniques such as liquid -liquid extraction (LLE) [11,13] and SPE [4,16,18]. Restricted access materials (RAM) have been used by excluding macromolecules from the matrix while selectively retaining the hydrophobic micromolecules [12,20].…”

Section: Introductionmentioning

confidence: 99%

Development of a validated HPLC method for the determination of four penicillin antibiotics in pharmaceuticals and human biological fluids

Samanidou¹,

Evaggelopoulou

Papadoyannis

2006

J. Sep. Sci.

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A quantitative method for the determination of four penicillin antibiotics, amoxicillin (AMO), oxacillin (OXA), cloxacillin (CLO), and dicloxacillin (DICLO), has been developed. Separation was achieved on an Inertsil ODS-3 (250 x 4 mm, 5 microm) column after selective extraction of penicillin drugs from biological matrices by means of SPE. Gradient elution with a mobile phase consisting of 0.1% TFA (pH 1) and ACN, and PDA detection with monitoring at 240 nm was applied. Salicylic acid (5 ng/microL) was used as the internal standard. RP-8 Adsorbex Merck cartridges provided high absolute recoveries (98-101%). The developed method was fully validated in terms of selectivity, linearity, accuracy, precision, stability, and sensitivity. Repeatability (n = 8) and between-day precision (n = 8) revealed RSD <10%. Recoveries from biological samples ranged from 91 to 103%. The detection limits were estimated as 3.3 ng for AMO, OXA, and CLO, and 6.6 for DICLO in blood plasma. LOD in whole blood and urine was 6.6 ng. Injection volume was 20 microL. The method was applied to commercially available AMO containing pharmaceuticals and spiked biological matrices. The method was also applied to biological samples after AMO oral administration, where the drug was successfully identified and quantified.

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Determination of eight penicillins in serum from cattle and pigs by generic HPLC method

Cited by 10 publications

References 26 publications

Identification, Isolation, and Characterization of a New Degradation Impurity in Nafcillin Sodium

Identification, Isolation, and Characterization of a New Degradation Impurity in Nafcillin Sodium

Development and validation of an HPLC method for the determination of seven penicillin antibiotics in veterinary drugs and bovine blood plasma

Development of a validated HPLC method for the determination of four penicillin antibiotics in pharmaceuticals and human biological fluids

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