High Performance Liquid Chromatography Determination of Fentin Acetate Residue in Beet and Soil

2012 ◽  
Vol 550-553 ◽  
pp. 1173-1176
Author(s):  
Hui Qing Sun ◽  
Yi Qiang Li ◽  
Guang Jun Xu ◽  
Xiao Zhen ◽  
Jin Li Xu ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Detectable Level ◽  
Relative Standard ◽  
External Standard ◽  
Detectable Concentration ◽  
Acid Aqueous Solution ◽  
Standard Calibration

Abstract. [Aims] A high performance liquid chromatography (HPLC) was presented for determination of fentin acetate residue in beet and soils. [Methods] Fentin acetate was extracted from beet plants and soils with hydrochloric acid and acetonitrile, followed by a second extraction in dichloromethane, purified by acid aluminium oxide with methanol eluting, then dissolved by concentration and dilution with acetoneitrile. A HPLC with UV detection at 220 nm and a Waters Sun FireTM-C18 column, which was eluted with methanol and 0.5% phosphoric acid aqueous solution and was used based on an external standard calibration curve. [Results] The results showed that the average recoveries were 88.4-95.6% for beet plants and 91.2-91.8% for soils. The relative standard deviations were 2.0-4.5% and 4.3-5.3% respectively. The minimum detectable level was 1.6×10-10g, the lowest detectable concentration was 0.02mg/kg. [Conclusions] The method is convenient and can meet the requirement of residual analysis and also provide reference for other crops.

scholarly journals A Selective High-Performance Liquid Chromatography Method for the Determination of Reboxetine in Bulk Drug and Tablets

2006 ◽  
Vol 89 (6) ◽  
pp. 1552-1556
Author(s):  
ArmaĞan Önal ◽  
Olcay SaĞiri ◽  
S Müge Çetin ◽  
Sidika Toker
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Depressive Disorders ◽  
Degradation Products ◽  
Severe Depression ◽  
Hplc Method ◽  
Chromatography Method ◽  
Relative Standard

Abstract Reboxetine is used as a selective noradrenaline reuptake inhibitor for the treatment of major depressive disorders. It is effective in the treatment of severe depression and safer to use than traditional tricyclic antidepressants. In this study, a novel, simple, and rapid stability-indicating high-performance liquid chromatography (HPLC) method for reboxetine methansulfonate was successfully developed and validated for the assay of tablets. The method was used to quantify reboxetine in tablets; it employed a C18 column (150 4.6 mm id) with an isocratic mobile phase consisting of methanolphosphate buffer (pH 7, 0.02 M; 55 + 45, v/v) at a flow rate of 1.0 μmL/min. Reboxetine was detected by an ultraviolet detector at 277 nm. The retention time of reboxetine was about 4.5 min. The developed HPLC method was validated with respect to linearity, precision, sensitivity, accuracy, and selectivity. The method was linear over the concentration range 150 g/mL (r 0.9999). The limits of detection and the quantitation of reboxetine were 0.1 and 0.3 μg/mL, respectively. The relative standard deviation values for intraday and interday precision were 0.781.01 and 1.081.37%, respectively. Selectivity was validated by subjecting a stock solution of reboxetine to neutral, acid, and alkali hydrolysis, as well as oxidation, dry heat treatment, and photodegradation. The peaks of the degradation products did not interfere with the peak of reboxetine. The results indicated that the proposed method could be used in a stability assay. The proposed method was successfully applied to the determination of reboxetine in tablets. Excipients present in the tablets did not interfere with the analysis.

Determination of Nitrate in Water by HPLC

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).

scholarly journals Development and validation of reversed phase high performance liquid chromatography (RP-HPLC) for quantification of captopril in rabbit plasma

2020 ◽  
Author(s):  
Muhammad Fawad Rasool ◽  
Umbreen Fatima Qureshi ◽  
Nazar Muhammad Ranjha ◽  
Imran Imran ◽  
Mouqadus Un Nisa ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Rabbit Plasma ◽  
Rp Hplc ◽  
Relative Standard

AbstractTh accurate rapid, simple and selective reversed phase high performance liquid chromatography (RP-HPLC) has been established and validated for the determination of captopril (CAP). Chromatographic separation was accomplished using prepacked ODSI C18 column (250 mm × 4.6 mm with 5 μm particle size) in isocratic mode, with mobile phase consisting of water: acetonitrile (60:40 v/v), pH adjusted to 2.5 by using 85% orthophosphoric acid at a flow rate of 1 mL/min and UV detection was performed at 203 nm. RP-HPLC method used for the analysis of CAP in mobile phase and rabbit plasma was established and validated as per ICH-guidelines. It was carried out on a well-defined chromatographic peak of CAP was established with a retention time of 4.9 min and tailing factor of 1.871. The liquid–liquid extraction method was used for extraction of CAP from the plasma. Excellent linearity (R2 = 0.999) was shown over range 3.125–100 µg/mL with mean percentage recoveries ranges from 97 to 100.6%. Parameters of precision and accuracy of the developed method meet the established criteria. Intra and inter-day precision (% relative standard deviation) study was also performed which was less than 2% which indicate good reproducibility of the method. The limit of detection (LOD) and quantification for the CAP in plasma were 3.10 and 9.13 ng/mL respectively. The method was suitably validated and successfully applied to the determination of CAP in rabbit plasma samples.

High Performance Liquid Chromatography with Fluorescence and Ultraviolet Detection of Polynuclear Aromatic Hydrocarbons in Barley Malt

1982 ◽  
Vol 65 (6) ◽  
pp. 1395-1402
Author(s):  
Frank L Joe ◽  
Jean Salemme ◽  
Thomas Fazio
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Aromatic Hydrocarbons ◽  
High Performance ◽  
Polynuclear Aromatic Hydrocarbons ◽  
Alumina Column ◽  
Reverse Phase ◽  
Barley Malt ◽  
Relative Standard

Abstract A simple, rapid method has been developed for the separation and determination of polynuclear aromatic hydrocarbons (PAHs) in barley malt. An ultrasonic- cyclohexane extraction method was used to separate the PAHs from ground barley malt. The cyclohexane extracts were purified by chromatography through a water-deactivated silica gel-alumina column. The eluate from the column was concentrated and purified further by partitioning between dimethyl sulfoxide (DMSO) and cyclohexane. The DMSO extract was diluted with water and the PAHs were extracted back into cyclohexane. The cyclohexane extract was washed with water, dried through sodium sulfate, and evaporated, and the resulting residue was dissolved in 80% aqueous acetonitrile-methanol (1 + 1) and subjected to reverse phase high performance liquid chromatography. Thirty barley malt samples were analyzed using this procedure. Peaks having the same retention time as the carcinogen benzo(a)pyrene were isolated from 18 of the samples, and were equivalent to trace levels ranging from <0.1 to 0.2 ppb. Average recoveries of 11 PAHs, including benzo(a)pyrene, benzo(b)fluoranthene, indeno(l,2,3-cd)pyrene, and benz(a)anthracene, added to 25 g samples at 2.5 and 5 ppb, ranged from 78 to 97%, with a mean relative standard deviation of 6.6%.

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

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.

scholarly journals Liquid-liquid extraction combined with high performance liquid chromatography-diode array-ultra-violet for simultaneous determination of antineoplastic drugs in plasma

2011 ◽  
Vol 47 (2) ◽  
pp. 363-371 ◽  
Author(s):  
Ananda Lima Sanson ◽  
Suéllen Cristina Rennó Silva ◽  
Matheus Coutinho Gonçalves Martins ◽  
Alexandre Giusti-Paiva ◽  
Patrícia Penido Maia ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Liquid Extraction ◽  
Therapeutic Drug ◽  
Diode Array ◽  
Antineoplastic Drugs ◽  
Liquid Liquid Extraction ◽  
Relative Standard

A liquid-liquid extraction (LLE) combined with high-performance liquid chromatography-diode array detection method for simultaneous analysis of four chemically and structurally different antineoplastic drugs (cyclophosphamide, doxorubicin, 5-fluorouracil and ifosfamide) was developed. The assay was performed by isocratic elution, with a C18 column (5 µm, 250 x 4.6 mm) and mobile phase constituted by water pH 4.0- acetonitrile-methanol (68:19:13, v/v/v), which allowed satisfactory separation of the compounds of interest. LLE, with ethyl acetate, was used for sample clean-up with recoveries ranging from 60 to 98%. The linear ranges were from 0.5 to 100 µg mL-1, for doxorubicin and 1 to 100 µg mL-1, for the other compounds. The relative standard deviations ranged from 5.5 to 17.7%. This method is a fast and simple alternative that can be used, simultaneously, for the determination of the four drugs in plasma, with a range enabling quantification of the drugs in pharmacokinetics, bioequivalence and therapeutic drug-monitoring studies.

scholarly journals Determination of metoprolol in pure and pharmaceutical dosage forms by spectrofluorometry and high performance liquid chromatography

2011 ◽  
Vol 17 (1) ◽  
pp. 25-31 ◽  
Author(s):  
Bilal Yilmaz ◽  
Kadem Meral ◽  
Ali Asci ◽  
Yavuz Organer
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Solvent System ◽  
Dosage Forms ◽  
Content Uniformity ◽  
Pharmaceutical Dosage Forms ◽  
Relative Standard ◽  
Limit Of Quantitation

In this study, a new and rapid spectrofluorometry and high performance liquid chromatography (HPLC) methods were developed for determination of metoprolol in pure and pharmaceutical dosage forms. The solvent system, wavelength of detection and chromatographic conditions were optimized in order to maximize the sensitivity of both the proposed methods. The linearity was established over the concentration range of 50-4000 ng ml-1 for spectrofluorometry and 5.0-300 ng ml-1 for HPLC methods. The intra- and inter-day relative standard deviation (RSD) was less than 4.14 and 3.86% for spectrofluorometry and HPLC, respectively. Limit of quantitation was determined as 30 and 5.0 ng ml-1 for spectrofluorometry and HPLC, respectively. No interference was found from tablet excipients at the selected assay conditions. The methods were applied for the quality control of commercial metoprolol dosage forms to quantify the drug and to check the formulation content uniformity.

Determination of β -Sitosterol with Chemical Course and Material Applications in Jatropha Seed Oil by High Performance Liquid Chromatography

2012 ◽  
Vol 577 ◽  
pp. 69-72 ◽  
Author(s):  
Shu Yu Liu ◽  
Anaerguli Maihemuti
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Seed Oil ◽  
Reversed Phase ◽  
Analytical Recovery ◽  
Relative Standard ◽  
The Mean ◽  
Jatropha Seed

A simple and rapid high performance liquid chromatography (HPLC) assay was developed to identify and measure theβ-sitosterol with chemical course and material applications in jatropha seed oil. The stigmasterol was isolated with a good selectivity by HPLC employing reversed phase C18 columns. The components were separated by mobile phase of methanol-water (99/1, v/v) and detected at 205nm. The quantitation of the stigmasterol was reproducible and the method relative standard deviation is 1.1%. The mean analytical recovery was 96.2%.

Determination of Diflubenzuron Residues in Vegetables by UPLC-MS/MS

2014 ◽  
Vol 852 ◽  
pp. 266-269
Author(s):  
Xiao Fang Wang ◽  
Chun Liang Yang ◽  
Mao Fang Huang ◽  
Ming Yue Wang ◽  
Yu Bing Zha ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
High Performance ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass

The conditions for detecting residues of diflubenzuron in vegetables by ultra high performance liquid chromatography tandem mass spectrometry were studied. The target was extracted with acetonitrile for 2 min with a homogenizer. The extaction was purifide by a conditioned Florisil SPE cartridge, and then was detected by ultra high-performance liquid chromatography with tandem mass spectrometry. The average recovery was in the range from 87.8 %- 99.2 % at spike levels of 0.1, 1.0 and 10 mg/kg in vegetables, and relative standard deviations was in the range of 4.2 %-8.9 %. The proposed method is fast, simple, sensitive and accurate.

scholarly journals Optimasi dan Validasi Metode Penentuan Kadar Asam Glikolat dan Asam Laktat Dalam Krim Menggunakan Kromatografi Cair Kinerja Tinggi

2020 ◽  
Vol 16 (1) ◽  
pp. 10
Author(s):  
Devi Wulandari ◽  
Gusrizal Gusrizal ◽  
Titin Anita Zaharah
Keyword(s):  
High Performance Liquid Chromatography ◽  
Lactic Acid ◽  
Liquid Chromatography ◽  
High Performance ◽  
Glycolic Acid ◽  
Orthophosphoric Acid ◽  
Spiked Sample ◽  
Relative Standard ◽  
Uv Visible

<p>Telah dilakukan optimasi dan validasi metode penentuan asam glikolat dan asam laktat dalam krim menggunakan kromatografi cair kinerja tinggi. Pemisahan asam glikolat dan asam laktat dilakukan pada kolom fasa balik C-8menggunakan fasa gerak asam ortofosfat 0,1% dengan pH 3,5 dan detektor <em>UV-Visible</em>. Standar asam glikolat dan asam laktat dibuat dengan melarutkannya menggunakan asam ortofosfat 0,1% pH 3,5. Hasil eksperimen menunjukkan bahwa pada rentang konsentrasi 25 – 400 μg/mL, asam glikolat dan asam laktat memiliki kurva yang linear dengan koefisien korelasi masing-masing 0,9997 dan 0,9999. Uji presisi untuk larutan standar berkonsentrasi 100 µg/mL menghasilkan simpangan baku relatif sebesar 1,49% untuk asam glikolat dan 1,72% untuk asam laktat. Metode yang telah dioptimasi memberikan akurasi yang baik yang ditunjukkan oleh nilai perolehan kembali dari pengukuran tiga <em>spiked sample</em> dengan konsentrasi berbeda (50, 100, dan 150 μg/mL). Nilai perolehan kembali untuk masing-masing konsentrasi <em>spiked sample</em> adalah 97,12% ± 0,69; 98,76% ± 0,43; 100,80% ± 0,29 untuk asam glikolat dan 97,58% ± 0,39; 96,20% ± 0,68; 98,00% ± 0,38 untuk asam laktat. Batas deteksi dan batas kuantisasi untuk asam glikolat adalah 0,05 dan 0,17 μg/mL, sedangkan untuk asam laktat adalah 1,40 dan 4,67 μg/mL. Nilai kekasaran metode untuk asam glikolat pada hari pertama dan hari kedua adalah 1,43% dan 1,67%, sedangkan untuk asam laktat adalah 1,67% dan 1,25%. Metode yang telah dioptimasi dan divalidasi berpotensi untuk digunakan secara spesifik pada penentuan kadar asam glikolat dan asam laktat dalam krim.</p><p><strong>Optimization and Validation of Determination Methods of Glycolic Acid and Lactic Acid in Cream Using High-Performance Liquid Chromatography.</strong> A high-performance liquid chromatography analytical method for the determination of glycolic acid and lactic acid in creams has been optimized and validated. The separation was performed in a reverse phase C–8 column with a mobile phase of 0.1%, orthophosphoric acid at pH 3.5, and UV-Visible detector. The standard of glycolic acid and lactic acid was dissolved in 0.1% orthophosphoric acid at pH 3.5. The experimental results showed that in the concentration range of 25–400 μg/mL, glycolic acid and lactic acid showed a linear curve with a correlation coefficient of 0.9997 and 0.9999, respectively. The precision test for standard solutions containing 100 µg/mL resulted in a relative standard deviation of 1.49% for glycolic acid and 1.72% for lactic acid. The optimized method provided good accuracy indicated by the recovery of the measurement of three spiked samples in different concentrations (50, 100, and 150 μg/mL). The recovery for each concentration of the spiked sample was 97.12% ± 0.69; 98.76% ± 0.43; 100.80% ± 0.29 for glycolic acid and 97.58% ± 0.39; 96.20% ± 0.68; 98.00% ± 0.38 for lactic acid. The limit of detection and limit of quantization for glycolic acid was 0.05 and 0.17 μg/mL, and for lactic acid was 1.40 and 4.67 μg/mL. The ruggedness of the method for glycolic acid on the first day and second day was 1.43% and 1.67%, while for lactic acid, it was 1.67% and 1.25%. The method that has been optimized and validated shows the potential to be used specifically for the determination of glycolic acid and lactic acid in the cream.</p>

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