scholarly journals Determination of Total Avermectin B1 and 8,9-Z-Avermectin B1 Residues in Wine by Liquid Chromatography

1996 ◽  
Vol 79 (5) ◽  
pp. 1158-1161 ◽  
Author(s):  
Janice A Cobin ◽  
Nelson A Johnson
Keyword(s):  
Liquid Chromatography ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Signal To Noise Ratio ◽  
Reversed Phase ◽  
Liquid Chromatographic Method ◽  
Limit Of Quantitation ◽  
Phase Liquid ◽  
Liquid Chromatographic

Abstract A liquid chromatographic method was developed and validated for determination of avermectin Bi and 8,9-Z-avermectin B1 residues in wine. The sample is extracted with hexane-acetonitrile and the hexane layer containing the avermectins is concentrated/ purified on an aminopropyl solid-phase extraction (SPE) column. The purified extract is derivatized with trifluoroacetic anhydride and the derivatized avermectins are analyzed by reversed-phase liquid chromatography with fluorescence detection. Recoveries of avermectins from wine fortified with approximately 1-25 ng/g avermectin B1a or 8,9-Zavermectin B1a averaged 88 and 102%, respectively. The limit of quantitation is 1 ng/g (signal-to-noise ratio [S/N] > 10) and the limit of detection is 0.5 ng/g (S/N > 3) for each analyte. This procedure provides a simple, rapid, and sensitive method for monitoring the total amount of avermectin residues in wine.

Liquid Chromatographic Method for Rapid Determination of Total Avermectin B1 and 8,9-Z-Avermectin B1 Residues in Apples

1995 ◽  
Vol 78 (2) ◽  
pp. 419-422 ◽  
Author(s):  
Janice A Cobin ◽  
Nelson A Johnson
Keyword(s):  
Chromatographic Method ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Rapid Determination ◽  
Reversed Phase ◽  
Extraction Column ◽  
Liquid Chromatographic Method ◽  
Limit Of Quantitation ◽  
Liquid Chromatographic

Abstract A liquid chromatographic method has been developed and validated for the rapid determination of avermectin B1 and 8,9-Z-avermectin B1 residues in apples. The avermectins are extracted from the crop matrix with an acetonitrile–water–hexane mixture; the extract is cleaned up on an aminopropyl solid-phase extraction column. The avermectins are derivatized with trifluoroacetic anhydride and analyzed by reversed-phase liquid chromatography with fluorescence detection. Recoveries of avermectins from apples fortified with about 2–77 ppb avermectin B1a or 2-27 ppb 8,9-Z-avermectin B1a averaged 85%. The limit of quantitation is 2 ppb (signal- to-noise [S/N] ratio, 12) and the limit of detection is 1 ppb (S/N ratio, 6) for each analyte. The assay is a simple, rapid, and sensitive method for monitoring the total amount of avermectin residues in apples.

Liquid Chromatographic Method for Determination of Total Avermectin Bi and 8,9-Z-Avermectin B1 Residues in Hops

1996 ◽  
Vol 79 (2) ◽  
pp. 503-507 ◽  
Author(s):  
Janice A Cobin ◽  
Nelson A Johnson
Keyword(s):  
Chromatographic Method ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Signal To Noise Ratio ◽  
Extraction Column ◽  
Assay Procedure ◽  
Liquid Chromatographic Method ◽  
Limit Of Quantitation ◽  
Liquid Chromatographic

Abstract A liquid chromatographic method has been developed and validated for determination of avermectin B1 and 8,9-Z-avermectin B1 residues in dried hops. The dried hops are rehydrated and subsequently extracted with a methanol-water mixture.The aver- mectins are partitioned into hexane and the hexane extract is concentrated (purified) on an amino- propyl solid-phase extraction column. The purified extract is derivatized with trifluoroacetic anhydride, and the derivatized avermectins are analyzed by re versed-phase liquid chromatography with fluorescence detection. Recoveries of the avermectins fromdried hops fortified with approximately 51000 ng/g avermectin B1a or 8,9-Z-avermectin B1a ranged from 73 to 108% with an overall average recovery of 95%. The limit of quantitation is 5 ng/g (signal-to-noise ratio [S/N] > 10), and the limit of detection is 2 ng/g (S/N > 3) for each analyte. The assay procedure provides a simple, rapid, and sensitive method for monitoring the total avermectin residues in hops.

scholarly journals Chlortetracycline, Oxytetracycline, and Tetracycline in Edible Animal Tissues, Liquid Chromatographic Method: Collaborative Study

1996 ◽  
Vol 79 (2) ◽  
pp. 405-417 ◽  
Author(s):  
James D MacNeil ◽  
Valerie K Martz ◽  
Gary O Korsrud ◽  
Craig D C Salisbury ◽  
Hisao Oka ◽  
...  
Keyword(s):  
Chromatographic Method ◽  
Solid Phase ◽  
Collaborative Study ◽  
Reversed Phase ◽  
Animal Tissues ◽  
Liquid Chromatographic Method ◽  
Phase Liquid ◽  
Tetracycline Residues ◽  
Liquid Chromatographic

Abstract Thirteen laboratories analyzed samples of edible animal tissues for tetracycline residues. The method included extraction of analytes into buffer, elution from a C18 solid-phase extraction (SPE) cartridge, and reversed-phase liquid chromatographic (LC) analysis, including use of a confirmation column. An additional laboratory, using an alternative LC assay based on a different sample cleanup, also analyzed the samples. Results showed the 2 methods are comparable. The LC method for determination of cholortetracycline, oxytetracycline, and tetracycline in edible animal tissues has been adopted by AOAC INTERNATIONAL. Results from 13 laboratories indicate that the method under study provides generally better results at the higher concentrations tested than at concentrations near the detection limit and that there is less problem with interferences in muscle tissue than in kidney. The method can achieve reliable results for analytes and matrixes studied at concentrations from 0.1 to 0.6 ppm and above, depending on the analyte-matrix combination, with generally better performance to be expected with muscle than with kidney. The poorer performance for fortified samples, particularly kidney, was attributed to additional homogenization steps required to prepare these samples. Recovery of analytes from different

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 HPLC determination of Escitalopram in tablet dosage forms

Pharmacia ◽  
2022 ◽  
Vol 69 (1) ◽  
pp. 21-24
Author(s):  
Stefan Balkanski
Keyword(s):  
Mobile Phase ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Dosage Forms ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Phase Liquid ◽  
Tablet Dosage ◽  
Liquid Chromatographic

Purpose: A simple, specific, precise, and accurate reversed phase liquid chromatographic (RP-LC) method has been developed for the determination of Escitalopram in tablet dosage form. Methods: The chromatographic separation was achieved on a LiChrosorb C18, 250 mm x 4.6 mm, 5 μm column at a detector wavelength of 270 nm and a flow rate of 1.0 ml/min. The mobile phase was composed of methanol, acetonitrile (70:30 v/v). The retention time of Escitalopram was 5.49 min. The method was validated for the parameters like specificity, linearity, precision, accuracy, limit of quantitation and limit of detection. Results: The method was found to be specific as no other peaks of impurities and excipients were observed. The square of correlation coefficient (R2) was 0.9999 while relative standard deviations were found to be <2.0%. Conclusion: The proposed RP-LC method can be applied for the routine analysis of commercially available formulations of Escitalopram.

scholarly journals Determination of Lincomycin Residue in Salmon Tissues by Ion-Pair Reversed-Phase Liquid Chromatography with Electrochemical Detection

1996 ◽  
Vol 79 (4) ◽  
pp. 839-843 ◽  
Author(s):  
Wenhong Luo ◽  
Eugene B Hansen ◽  
Catharina Y W Ang ◽  
Harold C Thompson
Keyword(s):  
Liquid Chromatography ◽  
Electrochemical Detection ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Reversed Phase ◽  
Ion Pair ◽  
Water Soluble ◽  
Reversed Phase Liquid Chromatography ◽  
Limit Of Quantitation ◽  
Phase Liquid

Abstract A method is described for detecting and quantitating lincomycin residue in salmon muscle and skin tissues by ion-pair reversed-phase liquid chromatography (LC) with electrochemical detection at +0.9 V. Lincomycin was extracted from tissues by homogenizing with 0.01 M KH2PO4 buffer (pH 4.5) and centrifuging the mixture. Water-soluble proteins were precipitated by adding sodium tungstate and sulfuric acid and removed by cent r if u gat ion. The buffer extract was then passed through a C18 solid-phase extraction cartridge. Lincomycin was eluted with 50% acetonitrile in water, and the eluate containing lincomycin was extracted with ethyl acetate. After the solvent had evaporated, the residue was redissolved in mobile phase and analyzed by LC. The method had a limit of detection of 7 ng/g lincomycin for salmon muscle and 12 ng/g for salmon skin. The limit of quantitation was 17 ng/g for salmon muscle and 24 ng/g for salmon skin. Average recoveries of lincomycin spiked at 50,100, and 200 ng/g were ≥85% for salmon muscle and ≥80% for salmon skin.

Simultaneous Liquid Chromatographic Determination of Fenamiphos and Its Metabolites in Soil

1992 ◽  
Vol 75 (1) ◽  
pp. 62-65 ◽  
Author(s):  
R Khazanchi ◽  
S Walia ◽  
S K Handa
Keyword(s):  
Chromatographic Method ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Chromatographic Determination ◽  
Reversed Phase ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic Determination ◽  
Phase Liquid ◽  
Liquid Chromatographic

Abstract A reversed-phase liquid chromatographic method has been developed for the determination of fenamiphos and the metabolites fenamiphos sulfoxide, fenamiphos sulfone, 3-methyl-4-(methylthlo)- phenol, and 3-methyl-4-(methylsulflnyl)phenol. Trace quantities of the nematlclde and Its metabolites In soil can be determined simultaneously. The limit of detection of the method was 5 ppm. Recoveries of fenamiphos and Its degradation products at fortification levels of 25,50, and 100 ppm ranged from 99.2 to 100.8%. Standard deviations ranged from 0.29 to 0.70 ppm.

scholarly journals Application of HPLC for the Simultaneous Determination of Paracetamol, Chlorzoxazone, and Nimesulide in Pharmaceutical Dosage Form

2012 ◽  
Vol 2012 ◽  
pp. 1-8 ◽  
Author(s):  
Snehal J. More ◽  
Suparna S. Tandulwadkar ◽  
Ajinkya R. Nikam ◽  
Atul S. Rathore ◽  
L. Sathiyanarayanan ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Dosage Form ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Control Analysis ◽  
Pharmaceutical Dosage Form ◽  
Limit Of Quantitation ◽  
Phase Liquid ◽  
Liquid Chromatographic

A simple, precise, and accurate reversed-phase liquid chromatographic method has been developed for the simultaneous determination of paracetamol (PCM), chlorzoxazone (CHZ), and nimesulide (NIM) in pharmaceutical dosage form. The chromatographic separation was achieved on a Thermo Hypersil GOLD C18 column (250 × 4.6 mm i.d., 5 μm particle size). The mobile phase consisted of water : acetonitrile (55 : 45 v/v). The flow rate was set to 1.2 mL min−1 and UV detection was carried out at 275 nm. The retention time () for PCM, CHZ, and NIM was found to be 2.69 ± 0.02, 4.61 ± 0.01, and 9.55 ± 0.02 min, respectively. The validation of the proposed method was carried out for linearity, precision, robustness, limit of detection, limit of quantitation, specificity, and accuracy. The linear dynamic ranges were 32.5–65.0 μg mL−1 for PCM, 37.5–75.0 μg mL−1 for CHZ, and 10.0–20.0 μg mL−1 for NIM. The developed method can be used for routine quality control analysis of titled drugs in pharmaceutical dosage form.

scholarly journals Validated Reversed-Phase Liquid Chromatographic Method with Gradient Elution for Simultaneous Determination of the Antiviral Agents: Sofosbuvir, Ledipasvir, Daclatasvir, and Simeprevir in Their Dosage Forms

Molecules ◽  
2020 ◽  
Vol 25 (20) ◽  
pp. 4611
Author(s):  
Essam Ezzeldin ◽  
Nisreen F. Abo-Talib ◽  
Marwa H. Tammam ◽  
Yousif A. Asiri ◽  
Abd El-Galil E. Amr ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Chromatographic Method ◽  
Limit Of Detection ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Dosage Forms ◽  
Liquid Chromatographic Method ◽  
Phase Liquid ◽  
Liquid Chromatographic

A simple, rapid, sensitive, and precise reversed-phase liquid chromatographic method was developed and validated for the simultaneous determination of four direct-acting antivirals, sofosbuvir (SF), ledipasvir (LD), declatasvir (DC), and simeprevir (SM), in their respective pharmaceutical formulations. Effective chromatographic separation was achieved on an Agilent Eclipse plus C8 column (250 mm × 4.6 mm, 5 µm) at 40 °C with gradient elution using a mobile phase composed of acetonitrile:phosphate buffer (pH 6.5). The quantification of SF and DC was based on peak area measurements at 260 nm, while the quantification of LD and SM was achieved at 330 nm. The linearity was acceptable from 1.0 to 20.0 μg/mL for the studied drugs, with correlation coefficients >0.999. The analytical performance of the newly proposed HPLC procedure was thoroughly validated according to ICH guidelines in terms of linearity, precision (RSD%, 0.39–1.57), accuracy (98.05–101.90%), specificity, limit of detection (LOD) (0.022–0.039 μg/mL), limit of quantification (LOQ) (0.067–0.118 μg/mL), and robustness. The validated HPLC method was successfully used to analyze the abovementioned drugs in their pure and dosage forms without interference from common excipients present in commercial formulations.

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