Multiresidue Determination of Fluoroquinolones in Shrimp by Liquid Chromatography-Fluorescence-Mass Spectrometryn

Abstract An efficient multiresidue method for analysis of fluoroquinolones in shrimp has been developed in which quantitation by fluorescence and confirmation by Multiple Stage Mass Spectrometry (MSn) is achieved simultaneously. In this method, shrimp tissue is extracted with ammoniacal acetonitrile and the extract is defatted and then evaporated. After dissolution in basic phosphate buffer, fluoroquinolones in the extract are separated by liquid chromatography and quantitated, taking advantage of their intense fluorescence. Eluate from the fluorescence detector enters the MSn, which allows for confirmation by monitoring ratios of 2 prominent product ions in the MS3 or MS2 spectrum. Using this method, 8 fluoroquinolones have been analyzed in shrimp samples fortified at 10, 25, 50, or 100 ppb levels. Recoveries for desethyleneciprofloxacin, norfloxacin, ciprofloxacin, danofloxacin, enrofloxacin, orbifloxacin, sarafloxacin, and difloxacin ranged from 75 to 92%, with relative standard deviation values of <6%. The limits of quantitation ranged from 0.1 to 1 ng/g. Enrofloxacin and ciprofloxacin were also successfully determined in enrofloxacin-incurred shrimp using this method.

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Evaluation of Serum as a Potential Matrix for Multiresidue Determination of Fluoroquinolone Antibiotics in Chicken Using Liquid Chromatography-Fluorescence-Mass Spectrometryn

Journal of AOAC International ◽

10.1093/jaoac/90.6.1716 ◽

2007 ◽

Vol 90 (6) ◽

pp. 1716-1723 ◽

Cited By ~ 6

Author(s):

Marilyn J Schneider ◽

Ixchel Reyes-Herrera ◽

Dan J Donoghue

Keyword(s):

Mass Spectrometry ◽

Liquid Chromatography ◽

Phosphate Buffer ◽

Chicken Serum ◽

Fluoroquinolone Antibiotics ◽

Relative Standard ◽

Potential Matrix ◽

Multiresidue Determination ◽

The U.S

Abstract An efficient multiresidue method was successfully applied to the determination of fluoroquinolones (FQs) in chicken serum. In this method, FQs are extracted from matrix with ammoniacal acetonitrile, and the extracts are defatted and then evaporated. After addition of basic phosphate buffer and filtration, the samples are analyzed by liquid chromatography-fluorescence-mass spectrometryn (multiple mass spectrometry; MSn). This approach allows for simultaneous quantitation (fluorescence) and confirmation (MSn) of the FQs. Using this method, 8 FQs were determined in fortified chicken serum at levels of 10, 20, 50, and 100 ng/g. Recoveries ranged from 7199, with excellent relative standard deviations (<10). Limits of quantitation for the FQs ranged from 0.055 ng/g. Confirmation was achieved by comparison of MS2 or MS3 product ion ratios with those of standard FQ samples. These quantitative and confirmatory results were compared with those obtained for muscle using this approach. Serum and muscle samples from enrofloxacin-dosed chickens were also analyzed with this method. The results show that enrofloxacin can be determined in both serum and muscle of chickens dosed at a level formerly approved by the U.S. Food and Drug Administration, for up to at least 48 h after withdrawal from dosing, and suggest that serum can provide an efficient matrix for monitoring FQ levels in chicken.

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Liquid Chromatographic Determination of Ampicillin Residues in Porcine Muscle Tissue by a Multipenicillin Analytical Method: European Collaborative Study

Journal of AOAC International ◽

10.1093/jaoac/85.4.889 ◽

2002 ◽

Vol 85 (4) ◽

pp. 889-900 ◽

Cited By ~ 1

Author(s):

Eric Verdon ◽

Pierric Couëdor ◽

Pierre Maris ◽

Michel Laurentie ◽

P Batjoens ◽

...

Keyword(s):

Mass Spectrometry ◽

Standard Deviation ◽

Relative Standard Deviation ◽

Muscle Tissue ◽

Phosphate Buffer ◽

Collaborative Study ◽

Porcine Muscle ◽

Relative Standard ◽

Liquid Chromatographic

Abstract A collaborative study involving 14 laboratories was conducted to determine residues of ampicillin in porcine muscle tissue by using a liquid chromatographic method developed for multipenicillin analysis that can quantitate 8 penicillin compounds (benzylpenicillin, phenoxymethylpenicillin, ampicillin, amoxicillin, nafcillin, oxacillin, cloxacillin, and dicloxacillin) at trace levels in muscle tissue. This method involves extraction of the penicillins with phosphate buffer, pH 9, followed cleanup and concentration on a C18 solid-phase extraction column and reaction with benzoic anhydride at 50°C and with 1,2,4-triazole and mercury(II) chloride solution, pH 9.0, at 65°C. The derivatized compounds are eluted isocratically on a C8 column with a mobile phase of acetonitrile and phosphate buffer (pH 6; 0.1M) containing sodium thiosulfate and the ion-pair reagent tetrabutylammonium hydrogen sulfate. The penicillins are detected by UV absorption at 325 nm. The limit of detection and the limit of determination (quantitation) of the method were calculated to be approximately 3–5 and 25 μg/kg, respectively, in accordance with the criteria of European Union (EU) Decision No. 93/256/EEC. In this first interlaboratory study, collaborators were instructed to monitor 4 different penicillin compounds (benzylpenicillin, phenoxymethylpenicillin, ampicillin, and amoxicillin) by analyzing 8 blind samples of muscle tissue in triplicate. These samples were prepared from 2 materials containing different concentrations of incurred ampicillin (63.5 μg/kg for material No. 1 and 358.1 μg/kg for material No. 2) and 1 blank material. The repeatability relative standard deviation and the reproducibility relative standard deviation were 10.2 and 17.4%, respectively, for material No. 1 and 7.0 and 16.0%, respectively, for material No. 2. These results demonstrate that the method is suitable for the determination of ampicillin residues in muscle tissue at the EU maximum residue limit (50 μg/kg) and above. However, the identification of positives by this procedure may need additional confirmation by techniques with greater specificity, such as liquid chromatography combined with mass spectrometry, or tandem mass spectrometry. Investigations regarding the basis of interlaboratory testing studies will further demonstrate the suitability of multiresidue methodology for detecting and quantitating other compounds in the family of penicillin antibiotics.

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Multiresidue Determination of Quinolone and Fluoroquinolone Antibiotics in Fish and Shrimp by Liquid Chromatography/Tandem Mass Spectrometry

Journal of AOAC International ◽

10.1093/jaoac/90.2.604 ◽

2007 ◽

Vol 90 (2) ◽

pp. 604-612 ◽

Cited By ~ 44

Author(s):

Guy Dufresne ◽

Andre Fouquet ◽

Don Forsyth ◽

Sheryl A Tittlemier

Keyword(s):

Mass Spectrometry ◽

Liquid Chromatography ◽

Tandem Mass Spectrometry ◽

Solid Phase ◽

Tandem Mass ◽

Fluoroquinolone Antibiotics ◽

Relative Standard ◽

Liquid Chromatography Tandem Mass ◽

Multiresidue Determination

Abstract A multiresidue method was developed to measure low levels of 8 fluoroquinolones (norfloxacin, ofloxacin, danofloxacin, ciprofloxacin, desethylene ciprofloxacin, enrofloxacin, sarafloxacin, and difloxacin) and 4 quinolones (oxolinic acid, flumequine, nalidixic acid, and piromidic acid). Method detection limits range from 0.1 ng/g for quinolones to 0.4 ng/g for fluoroquinolones. Average recoveries range from 57 to 96%, depending on analyte and commodity; relative standard deviations are all less than 18%. The drugs are extracted from tissues using a mixture of ethanol and 1% acetic acid, diluted in aqueous HCl, and defatted by extraction with hexane. The compounds are further isolated using cation-exchange solid-phase extraction and measured using liquid chromatography with electrospray tandem mass spectrometry detection. The method has been evaluated and applied to the analysis of salmon, trout, and shrimp. Detectable residues were observed in 10 out of 73 samples, at concentrations ranging from 0.28 to 16 ng/g.

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SIMULTANEOUS DETERMINATION OF PARACETAMOL AND IBUPROFENE MIXTURES BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY

Indonesian Journal of Chemistry ◽

10.22146/ijc.21899 ◽

2010 ◽

Vol 3 (1) ◽

pp. 9-13 ◽

Cited By ~ 1

Author(s):

Sophi Damayanti ◽

Slamet Ibrahim ◽

Kurnia Firman ◽

Daryono H Tjahjono

Keyword(s):

High Performance Liquid Chromatography ◽

Liquid Chromatography ◽

Standard Deviation ◽

Retention Time ◽

Analytical Method ◽

Phosphate Buffer ◽

Mobile Phase ◽

High Performance ◽

Relative Standard

Analytical method for the determination of paracetamol and ibuprofene mixtures has been developed by High Performance Liquid Chromatography using C-18 column and acetinitrile - phosphate buffer pH = 4.5 (75:25) containing 0.075% sodium hexanesulfunate as a mobile phase. The detector was set at 215 nm. Using such conditions, retention time for paracetamol and ibuprofen was 4.89 and 7.11 min, respectively. The recovery for paracetamol and ibuprofen was found to be 101.07± 0.73% and 102.02 ± 1.58%, respectively. The detector limits of the method was 1.30 and 1.60 μg/mL with the relative standard deviation (RSD) 0.74 and 1.52% for paracetamol and ibuprofen, respectively. Keywords: paracetamol, ibuprofen, multi-component, validation, HPLC.

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Method Validation for Determination of Alkaloid Content in Goldenseal Root Powder

Journal of AOAC International ◽

10.1093/jaoac/86.3.476 ◽

2003 ◽

Vol 86 (3) ◽

pp. 476-483 ◽

Cited By ~ 12

Author(s):

Holly A Weber ◽

Matthew K Zart ◽

Andrew E Hodges ◽

Kellie D White ◽

Sarah M Barnes ◽

...

Keyword(s):

Mass Spectrometry ◽

Liquid Chromatography ◽

Standard Deviation ◽

Relative Standard Deviation ◽

Analytical Method ◽

Hydrastis Canadensis ◽

Extraction Solvent ◽

Relative Standard ◽

Oregon Grape

Abstract A fast, practical ambient extraction methodology followed by isocratic liquid chromatography (LC) analysis with UV detection was validated for the determination of berberine, hydrastine, and canadine in goldenseal (Hydrastis canadensis L.) root powder. The method was also validated for palmatine, a major alkaloid present in the possible bioadulterants Coptis, Oregon grape root, and bar-berry bark. Alkaloid standard solutions were linear over the evaluated concentration ranges. The analytical method was linear for alkaloid extraction using 0.3–2 g goldenseal root powder/100 mL extraction solvent. Precision of the method was demonstrated using 10 replicate extractions of 0.5 g goldenseal root powder, with percent relative standard deviation for all 4 alkaloids ≤1.6. Alkaloid recovery was determined by spiking each alkaloid into triplicate aliquots of neat goldenseal root powder. Recoveries ranged from 92.3% for palmatine to 101.9% for hydrastine. Ruggedness of the method was evaluated by performing multiple analyses of goldenseal root powder from 3 suppliers over a 2-year period. The method was also used to analyze Coptis root, Oregon grape root, barberry bark, and celandine herb, which are possible goldenseal bioadulterants. The resulting chromato-graphic profiles of the bioadulterants were significantly different from that of goldenseal. The method was directly transferred to LC with mass spectrometry, which was used to confirm the presence of goldenseal alkaloids tetrahydro-berberastine, berberastine, canadaline, berberine, hydrastine, and canadine, as well as alkaloids from the bioadulterants, including palmatine, jatrorrhizine, and coptisine.

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Determination of Nitrate in Water by HPLC

Applied Mechanics and Materials ◽

10.4028/www.scientific.net/amm.448-453.406 ◽

2013 ◽

Vol 448-453 ◽

pp. 406-408

Author(s):

Jing Liu ◽

Xiao Na Ji ◽

Qing Kai Ren ◽

Sheng Shu Ai ◽

Li Jun Wan ◽

...

Keyword(s):

High Performance Liquid Chromatography ◽

Liquid Chromatography ◽

Standard Deviation ◽

Relative Standard Deviation ◽

Recovery Rate ◽

High Performance ◽

Separation Efficiency ◽

Fast Analysis ◽

Relative Standard

We established a method fordetermination of nitrate in water by High Performance Liquid Chromatography(HPLC). The sample was analysed by HPLC-ADA and was quantitated by externalstandard method after being simply processed. This methd has the advantages ofhigh separation efficiency and fast analysis. The experiment result showed thatthe linearly dependent coefficient was0.994, the recovery rate was between 98.7%～105.7%,the relative standard deviation（RSD）wasless than 2.1 %, and the lowest detectable limit is 0.01ng (S/N=1.6).

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Gas-Liquid Chromatography of Trichlorfon in Soluble Powder Formulations

Journal of AOAC INTERNATIONAL ◽

10.1093/jaoac/57.5.1128 ◽

1974 ◽

Vol 57 (5) ◽

pp. 1128-1131

Author(s):

Phil B Bowman ◽

Peter W Dame

Keyword(s):

Liquid Chromatography ◽

Standard Deviation ◽

Relative Standard Deviation ◽

Trimethylsilyl Ether ◽

Gas Liquid Chromatography ◽

Mass Spectral ◽

Powder Formulation ◽

Relative Standard ◽

Quantitative Recovery

Abstract A procedure is described for the determination of trichlorfon in a soluble powder formulation by gas-liquid chromatography. Silylation prevents on-column degradation of trichlorfon to dichlorvos. The procedure provides quantitative recovery from the formulation as demonstrated by a spiking study. A relative standard deviation of less than 2% was obtained for 6 replicate assays of a single lot of formulation. The mass spectral fragmentations of trichlorfon and trichlorfon-trimethylsilyl ether are described.

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Liquid Chromatography–Tandem Mass Spectrometry for the Simultaneous Determination of Doxorubicin and its Metabolites Doxorubicinol, Doxorubicinone, Doxorubicinolone, and 7-Deoxydoxorubicinone in Mouse Plasma

Molecules ◽

10.3390/molecules25051254 ◽

2020 ◽

Vol 25 (5) ◽

pp. 1254 ◽

Cited By ~ 1

Author(s):

Won-Gu Choi ◽

Dong Kyun Kim ◽

Yongho Shin ◽

Ria Park ◽

Yong-Yeon Cho ◽

...

Keyword(s):

Mass Spectrometry ◽

Liquid Chromatography ◽

Tandem Mass Spectrometry ◽

Simultaneous Determination ◽

Tandem Mass ◽

Mouse Plasma ◽

Chromatography Tandem Mass Spectrometry ◽

Relative Standard ◽

Liquid Chromatography Tandem Mass

Doxorubicin, an anthracycline antitumor antibiotic, acts as a cancer treatment by interfering with the function of DNA. Herein, liquid chromatography-tandem mass spectrometry was for the first time developed and validated for the simultaneous determination of doxorubicin and its major metabolites doxorubicinol, doxorubicinone, doxorubicinolone, and 7-deoxydoxorubicinone in mouse plasma. The liquid–liquid extraction of a 10 μL mouse plasma sample with chloroform:methanol (4:1, v/v) and use of the selected reaction monitoring mode led to less matrix effect and better sensitivity. The lower limits of quantification levels were 0.5 ng/mL for doxorubicin, 0.1 ng/mL for doxorubicinol, and 0.01 ng/mL for doxorubicinone, doxorubicinolone, and 7-deoxydoxorubicinone. The standard curves were linear over the range of 0.5–200 ng/mL for doxorubicin; 0.1–200 ng/mL for doxorubicinol; and 0.01–50 ng/mL for doxorubicinone, doxorubicinolone, and 7-deoxydoxorubicinone in mouse plasma. The intra and inter-day relative standard deviation and relative errors for doxorubicin and its four metabolites at four quality control concentrations were 0.9–13.6% and –13.0% to 14.9%, respectively. This method was successfully applied to the pharmacokinetic study of doxorubicin and its metabolites after intravenous administration of doxorubicin at a dose of 1.3 mg/kg to female BALB/c nude mice.

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Determination of Patulin in Apple Juice by Liquid Chromatography

Journal of AOAC International ◽

10.1093/jaoac/89.1.139 ◽

2006 ◽

Vol 89 (1) ◽

pp. 139-143 ◽

Cited By ~ 20

Author(s):

Maria Helena Iha ◽

Myrna Sabino

Keyword(s):

Liquid Chromatography ◽

Standard Deviation ◽

Mobile Phase ◽

Apple Juice ◽

Array Detector ◽

Diode Array ◽

Diode Array Detector ◽

Relative Standard ◽

Precision Study

Abstract A method was developed and validated in-house for the determination of patulin (PAT), a toxic mold metabolite, in apple juice. The sample was extracted with ethyl acetatehexane and analyzed by liquid chromatography equipped with a C18 column and diode array detector. The mobile phase used for the quantification was waterethanol, at a flow rate of 0.5 mL/min. The method showed a mean recovery of 84.8%, the relative standard deviation obtained in the precision study was <7.7%, the quantification and detection limits were 7 and 3 μg/L, respectively, and the linear range for PAT in apple juice was 2.6650 μg/L. The ruggedness was evaluated by an intralaboratory experiment, in which 5 factors were studied, and only one was found to influence the observed results. The developed method is fast, practical, and simple; the solvents (except hexane) and reagents used were nontoxic. The results of the validation confirmed the efficiency of the method, which is sensitive enough to be used in studies required to quantify PAT in apple juice.

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Validation of HPLC Method for Determination of Histamine in Human Immunoglobulin Formulations

Journal of AOAC International ◽

10.1093/jaoacint/qsaa017 ◽

2020 ◽

Vol 103 (5) ◽

pp. 1223-1229

Author(s):

Michikazu Tanio ◽

Toru Nakamura ◽

Hideki Kusunoki ◽

Kyohei Ideguchi ◽

Kazuyuki Nakashima ◽

...

Keyword(s):

High Performance Liquid Chromatography ◽

Liquid Chromatography ◽

Standard Deviation ◽

High Performance ◽

Gradient Elution ◽

Hplc Method ◽

Human Immunoglobulin ◽

Histamine Dihydrochloride ◽

Relative Standard

Abstract Background Histamine fixed-immunoglobulin formulations, which consisted of 0.15 µg of histamine dihydrochloride and 12 mg of human immunoglobulin in a vial, are used for anti-allergic treatments, and controlling the amounts of histamine in the formulations is essential to avoid histamine intoxication. Objective A high-performance liquid chromatography (HPLC) method for determination of histamine contents of the formulations was established and validated. Methods Histamine extracted from the formulation was labeled with 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate and was analyzed by gradient elution HPLC with UV detection at 260 nm. Results The method showed linearity in the range 0.8–2.4 µM (R > 0.999), accuracy (100.1–105.8% recovery), and precision (relative standard deviation ≤ 1.93%). The validated method was applied for five lots of the pharmaceutical, and their histamine contents were determined to be 0.149–0.155 µg/vial. Conclusions These results indicated that the validated method is useful to control amounts of histamine in biopharmaceutical products. Highlights The HPLC method was developed for quantitative determination of histamine content of the histamine fixed-immunoglobulin formulations.

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