Analysis of Penicillin G in Milk by Liquid Chromatography

1994 ◽  
Vol 77 (3) ◽  
pp. 565-570 ◽  
Author(s):  
Joe O K Boison ◽  
Lily J-Y Keng ◽  
James D Macneil
Keyword(s):  
Liquid Chromatography ◽  
Detection Limit ◽  
Sodium Tungstate ◽  
Solid Phase ◽  
Internal Standard ◽  
Penicillin G ◽  
Penicillin V ◽  
Solid Phase Extraction Cartridge ◽  
Mercuric Chloride Solution ◽  
Liquid Chromatographic

Abstract A liquid chromatographic (LC) method that was previously developed for penicillin G residues in animal tissues has been adapted to milk and milk products. After protein precipitation with sodium tungstate, samples are applied to a C18 solid-phase extraction cartridge, from which penicillin is eluted, derivatized with 1,2,4-triazole-mercuric chloride solution, and analyzed by isocratic liquid chromatography (LC) on a C18 column with UV detection at 325 nm. Quantitation is done with reference to penicillin V as an internal standard. Penicillin G recoveries were determined to be >70% on standards fortified at 3-60 ppb. Accuracy approached 100% using the penicillin V internal standard. The detection limit for penicillin G residues was 3 ppb in fluid milk. Samples may be confirmed by thermospray/LC at concentrations approaching the detection limit of the UV method.

scholarly journals Determination of Penicillin G in Feeds by Liquid Chromatography with Solid-Phase Extraction

2005 ◽  
Vol 88 (3) ◽  
pp. 679-683 ◽  
Author(s):  
Matthew J Gramse ◽  
Paul E Jacobson
Keyword(s):  
Liquid Chromatography ◽  
Solid Phase Extraction ◽  
Solid Phase ◽  
Reversed Phase ◽  
Penicillin G ◽  
Phase Extraction ◽  
Solid Phase Extraction Cartridge ◽  
Relative Standard ◽  
Liquid Chromatographic

Abstract A liquid chromatographic method was developed for the determination of penicillin G in feeds. The method involves extraction of penicillin G with methanol, concentration under a stream of nitrogen, and cleanup using Phenomenex Strata-X solid-phase extraction cartridge. Analyte separation and quantification were achieved by gradient reversed-phase liquid chromatography and ultraviolet absorbance at 230 nm. Average spike recoveries for samples prepared at 3 spiking levels (25, 50, and 200 g/ton) were 96.3, 92.1, and 88.6%, respectively. The overall method precision at each of the 3 spiking levels was ≤5.39% relative standard deviation. The limits of detection and quantititation (g/ton formulation) were 3.89 and 13.0 g/ton, respectively.

Analysis of 5-Vinyl-l,3-Oxazolidine-2-Thione by Liquid Chromatography

1992 ◽  
Vol 75 (3) ◽  
pp. 529-536 ◽  
Author(s):  
Alain Quinsac ◽  
Daniel Ribaillier ◽  
Patrick Rollin ◽  
Michel Dreux
Keyword(s):  
Liquid Chromatography ◽  
Solid Phase ◽  
Internal Standard ◽  
Rapeseed Meal ◽  
Reversed Phase ◽  
Mercury Acetate ◽  
Phase Liquid ◽  
Biological Environment ◽  
Liquid Chromatographic

Abstract 5-Vlnyl-1,3-oxazolldlne-2-thlone (5-VOT) Is a goltrlgenlc compound released by enzymatic degradation of progoltrln, the major glucoslnolate occurring In rapeseed meal. A liquid chromatographic (LC) method for determination of 5-VOT in a biological environment Is presented. Complete extraction of 5-VOT has been carried out by complexatlon with phenyl mercury acetate under cyclohexanlc conditions, and then by decomplexation using an aqueous sodium thlosulfate solution. These reactions displace 5-VOT from an aqueous to an organic medium, and then back again to the aqueous condition, thus assuring high selectivity of the extraction. Precise quantitation of 5-VOT Is completed in 10 mln by reversed-phase liquid chromatography using an isocratic elutlon with UV detection and a specially made synthetic Internal standard. Concentration steps by solid-phase chromatography and evaporation can be introduced In the analytic procedure to lower the detection limit of 5-VOT in the sample used from 100 to 0.5 ppb. Using sow milk samples, the method was tested by small measured additions of 5-VOT. The recovery rate of the product was very good (>97%). Different phases used to achieve a sensitive, rapid, and precise method are described.

scholarly journals Confirmatory Determination of Six Penicillins in Honey by Liquid Chromatography/Electrospray Ionization–Tandem Mass Spectrometry

2004 ◽  
Vol 87 (1) ◽  
pp. 45-55 ◽  
Author(s):  
Jian Wang
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Electrospray Ionization ◽  
Solid Phase ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Penicillin G ◽  
Tandem Mass ◽  
Ionization Tandem Mass Spectrometry

Abstract A confirmatory method for 6 penicillin antibiotics (amoxicillin, ampicillin, penicillin G, oxacillin, cloxacillin, and dicloxacillin) in honey is presented that allows determination and confirmation of identity of the antibiotics at trace levels. The method includes the use of a stable isotope-labeled internal standard benzyl (d7-phenyl) penicillate and removal of sugar and other substances by solvent and solid-phase extraction. The honey extracts are then analyzed for penicillin residues by liquid chromatography/electrospray ionization–tandem mass spectrometry. Mass spectral acquisition was achieved in an electrospray positive ion mode by applying multiple reaction monitoring of 2 or 3 fragment ion transitions to provide a high degree of sensitivity and specificity. Typical recoveries of 6 penicillins at fortification levels of 6, 16, 40, and 80 μg/kg ranged from 51.4 to 132.9%. The recoveries varied with the individual penicillins and were affected by different honey matrixes. The ion ratios were consistent and could be used for confirmation of identity of the penicillins. The method limits of detection (μg/kg) were 0.25 for amoxicillin, 0.19 for ampicillin, 0.068 for penicillin G, 0.028 for oxacillin, 0.052 for cloxacillin, and 0.085 for dicloxacillin. The method limits of confirmation (μg/kg) were 0.44 for amoxicillin, 0.52 for ampicillin, 0.23 for penicillin G, 0.14 for oxacillin, 0.14 for cloxacillin, and 0.15 for dicloxacillin when a sample size of 5 g honey was used.

Sensitive Determination of Zearalenone and α-Zearalenol in Barley and Job's-Tears by Liquid Chromatography with Fluorescence Detection

1993 ◽  
Vol 76 (5) ◽  
pp. 1006-1009 ◽  
Author(s):  
Touicm Tanaka ◽  
Reiko Teshima ◽  
Hideharu Ikebuchi ◽  
Jun-Ichi Sawada ◽  
Tadao Terao ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Detection Limit ◽  
Fluorescence Detection ◽  
Reliable Method ◽  
Internal Standard ◽  
Reversed Phase ◽  
Job’S Tears ◽  
Sensitive Determination ◽  
Liquid Chromatographic

Abstract A sensitive and reliable method for liquid chromatographic (LC) determination of zearalenone and α-azearalenol in barley and Job's-tears was investigated. The method by which these toxins were determined involves addition of an internal standard (zearalenone 6'-oxime) to barley and Job's-tears samples. Extracts from grain samples were cleaned up by passage through chromatography on piperidinohydroxypropyl Sephadex LH-20 as a lipophilic gel. Individual toxins were resolved by LC on a reversed-phase (ODS) column with fluorescence detection. The detection limit is estimated to be 0.2 ng for zearalenone and α-zearalenol standards. Known amounts of zearalenone and α-azearalenol (25-1250 ng) were added to a barley sample (5 g). Average recoveries for α-zearalenol and zearalenone, respectively, ranged from 96 to 102% (mean CV, 3.6%) and from 96 to 103% (mean CV, 3.3%). This method is applicable to determination of α-zearalenol and zearalenone in barley and Job's-tears with satisfactory sensitivity and accuracy.

Determination of Penicillin G Residues in Edible Animal Tissues by Liquid Chromatography

1991 ◽  
Vol 74 (3) ◽  
pp. 497-501 ◽  
Author(s):  
Joe O Boison ◽  
Craig D C Salisbury ◽  
Wayne Chan ◽  
James D Macneil
Keyword(s):  
Liquid Chromatography ◽  
Limit Of Detection ◽  
Phosphate Buffer Solution ◽  
Internal Standard ◽  
Penicillin G ◽  
Extraction Column ◽  
Animal Tissues ◽  
Benzyl Penicillin ◽  
Penicillin V

Abstract An Improved method has been developed for the determination of benzyl penicillin In animal tissues. Tissues are fortified with a known amount of penicillin V (Internal standard) and extracted with water. The extract Is deproteinlzed with sulfuric acid and sodium tungstate, filtered, and concentrated on a conditioned C18 solid phase extraction column. Penicillin V and benzyl penicillin are then eluted from the column with 1 mL 60% acetonitrile-35% water-5% 0.2M phosphate buffer solution and derivatlzed with 1 mL 1,2,4-trlazole-mercuric chloride solution at 65°C for 30 min. An aliquot of this sample Is analyzed by reverse phase liquid chromatography with UV detection at 325 nm. The limit of detection is 5 μg/kg (ppb) penicillin G (8.4 lU/kg) In liver, kidney, and muscle tissues

Solid-phase extraction and liquid chromatography for improved assay of cyclosporine in whole blood or plasma.

1985 ◽  
Vol 31 (10) ◽  
pp. 1717-1720 ◽  
Author(s):  
P M Kabra ◽  
J H Wall ◽  
N Blanckaert
Keyword(s):  
Liquid Chromatography ◽  
Whole Blood ◽  
Present Method ◽  
Solid Phase ◽  
Internal Standard ◽  
Extraction Column ◽  
Phase Extraction ◽  
Analytical Recovery ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic

Abstract In this simple, precise, accurate, and specific isocratic liquid chromatographic procedure for determining cyclosporine, the cyclosporine is extracted from 1 mL of whole blood or from plasma, with 500 micrograms of cyclosporin D added per liter as internal standard, by elution from a Bond-ElutTM C18 extraction column with 300 microL of a mixture of ethanol and tetrahydrofuran. A 100-microL aliquot of the eluate, injected onto a cyano-phase analytical column, is eluted with a mixture of acetonitrile and pH 7.0 phosphate buffer at a flow rate of 1.0 mL/min and at 50 degrees C. Detection is at 210 nm. The chromatography is complete in less than 14.0 min. The method can measure less than 10.0 micrograms/L. Analytical recovery of cyclosporine added to whole blood ranged from 99 to 109% for concentrations up to 2000 micrograms/L. Between-run CVs ranged from 6.4 to 6.6%. None of numerous drugs and steroids tested interfered. Results by radioimmunoassay exceeded by 20 to 350% those measured by the present method.

scholarly journals High-performance liquid chromatographic determination of famotidine in human plasma using solid-phase column extraction

2003 ◽  
Vol 68 (11) ◽  
pp. 883-892 ◽  
Author(s):  
Dragica Zendelovska ◽  
Trajce Stafilov
Keyword(s):  
Human Plasma ◽  
High Performance ◽  
Solid Phase ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Water Ph ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

A rapid, specific and sensitive high-performance liquid chromatographic method for the determination of famotidine in human plasma has been developed. Famotidine and the internal standard were chromatographically separated from plasma components using a Lichrocart Lichrospher 60 RP select B cartridge for solid-phase separation with a mobile phase composed of 0.1 % (v/v) triethylamine in water (pH 3) and acetonitrile (92:8, v/v). UV detection was set at 270 nm. The calibration curve was linear in the concentration range of 10.0 ? 350.0 ng mL-1. The method was implemented to monitor the famotidine levels in patient samples.

scholarly journals Rapid and Sensitive Method for Quantitative Determination of Lopinavir and Ritonavir in Human Plasma by Liquid Chromatography- Tandem Mass Specrtometry

2009 ◽  
Vol 6 (1) ◽  
pp. 223-230 ◽  
Author(s):  
G. A. Temghare ◽  
S. S. Shetye ◽  
S. S. Joshi
Keyword(s):  
Liquid Chromatography ◽  
Human Plasma ◽  
Solid Phase ◽  
Internal Standard ◽  
Therapeutic Monitoring ◽  
Tandem Mass ◽  
Limit Of Quantification ◽  
Liquid Chromatography Tandem Mass ◽  
Sensitive Method

A rapid and sensitive liquid chromatography-mass spectrometric (LC-MS-MS) method for the simultaneous determination of lopinavir and ritonavir in human plasma using abacavir as internal standard has been developed and validated. Sample preparation of plasma involved solid phase extraction. Detection was performed using an Applied Biosystems Sciex API 2000 Mass spectrometer. The assay of lopinavir and ritonavir was linear over the range of 50 ng mL-1to 20000 ng mL-1and 20 ng mL-1to 3000 ng mL-1 respectively with a precision of <15% and accuracy in the range of 85-115%. The limit of quantification in plasma for lopinavir and ritonavir was 50 ng mL-1and 20 ng mL-1respectively. The described method has the advantage of being rapid and easy and it could be applied in therapeutic monitoring of these drugs in human plasma

scholarly journals Analytical Determination of Virginiamycin Drug Residues in Edible Porcine Tissues by LC-MS with Confirmation by LC-MS/MS

2009 ◽  
Vol 92 (1) ◽  
pp. 329-339 ◽  
Author(s):  
Joe Boison ◽  
Stephen Lee ◽  
Ron Gedir
Keyword(s):  
Solid Phase ◽  
Minor Component ◽  
Analytical Determination ◽  
Porcine Liver ◽  
Solid Phase Extraction Cartridge ◽  
Muscle Tissues ◽  
Dried Extract ◽  
A Minor ◽  
Liquid Chromatographic

Abstract A liquid chromatographic-mass spectrometric (LC-MS) method was developed and validated for the determination and confirmation of virginiamycin (VMY) M1 residues in porcine liver, kidney, and muscle tissues at concentrations 2 ng/g. Porcine liver, kidney, or muscle tissue is homogenized with methanolacetonitrile. After centrifugation, the supernatant is diluted with phosphate buffer and cleaned up on a C18 solid-phase extraction cartridge. VMY in the eluate is partitioned into chloroform and the aqueous upper layer is removed by aspiration. After evaporating the chloroform in the residual mixture to dryness, the dried extract is reconstituted in mobile phase and VMY is quantified by LC-MS. Any samples eliciting quantifiable levels of VMY M1 (i.e., at concentrations 2 ng/g) are subjected to confirmatory analysis by LC-MS/MS. VMY S1, a minor component of the VMY complex, is monitored but not quantified or confirmed.

scholarly journals Sensitive and Rapid Quantification of Busulfan in Small Plasma Volumes by Liquid Chromatography–Electrospray Mass Spectrometry

2001 ◽  
Vol 47 (8) ◽  
pp. 1437-1442 ◽  
Author(s):  
Thomas E Mürdter ◽  
Janet Coller ◽  
Alexander Claviez ◽  
Frank Schönberger ◽  
Ute Hofmann ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Therapeutic Drug Monitoring ◽  
Drug Monitoring ◽  
Internal Standard ◽  
Therapeutic Drug ◽  
High Dose ◽  
Selected Ion Monitoring ◽  
Hematopoietic Stem ◽  
Adults And Children ◽  
Liquid Chromatographic

Abstract Background: High-dose busulfan is widely used in conditioning regimens before hematopoietic stem cell transplantation in both adults and children. Large interindividual variability in pharmacokinetics after oral administration has been reported; therefore, therapeutic drug monitoring of busulfan may decrease the incidence of drug-related toxicity (for example, hepatic venoocclusive disease) and may also improve therapeutic efficacy. Methods: Busulfan concentrations were quantified using 200 μL of plasma and liquid–liquid extraction with diethyl ether after the addition of [2H8]busulfan as the internal standard. Separation and detection of busulfan and [2H8]busulfan were achieved with a LUNA C8 column (5 μm; 150 × 2 mm i.d.) at 30 °C, a HP 1100 liquid chromatography system, and a HP 1100 single-quadrupole mass spectrometer. Busulfan and [2H8]busulfan were detected as ammonium adducts in selected-ion monitoring mode at m/z 264.2 and 272.2, respectively. Results: The calibration curve was linear at 5–2000 μg/L busulfan. Intra- and interassay imprecision (CV) and bias were both &lt;11%. The limits of detection and quantification were 2 and 5 μg/L, respectively. Extraction recovery of busulfan was &gt;87%. Analysis of pharmacokinetics in four patients receiving high-dose busulfan indicated that minimum busulfan concentrations before the next dose were 405–603 μg/L, with no interference observed. Conclusions: The new rapid and sensitive liquid chromatographic–mass spectrometric assay is an appropriate method for quantification of busulfan in human plasma, making therapeutic drug monitoring of busulfan faster and easier in clinical practice.

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