High Performance Liquid Chromatographic Method for Simultaneous Determination of Residual Benomyl and Methyl 2-BenzimidazoIe Carbamate on Apple Foliage Without Cleanup

1980 ◽  
Vol 63 (6) ◽  
pp. 1291-1295
Author(s):  
Mikio Chiba ◽  
D F Veres

Abstract A simple HPLC method has been developed to individually determine residues of benomyl and MBC on apple leaves without cleanup. Sample leaves in a Mason jar are freeze-dried and tumbled for extraction in CHC13 containing 5000 μg n-propyl isocyanate/mL at 1°C. n-Butyl isocyanate is added to the extract at 5000 μg/mL, and 20 μL of the mixture is injected into the HPLC system. A Brownlee LiChrosorb silica gel column with a guard column is operated with a mixed mobile phase of chloroform-hexane (4+1) saturated with water. MBC, present as a degradation compound of benomyl, is identified as methyl 1 – (n – propylcarbamoyl) – 2 – benzimidazole carbamate (MBC-n-PIC derivative). At 280 nm, both benomyl and MBC-n-PIC can be detected with a UV detector at a level of 0.2 ppm in apple leaves.

2011 ◽  
Vol 47 (2) ◽  
pp. 261-268 ◽  
Author(s):  
Elisabete de Almeida Barbosa Antunes ◽  
Felipe Rebello Lourenço ◽  
Terezinha de Jesus Andreoli Pinto

A high-performance liquid chromatographic method employing pre-column derivatization with o-phthalaldehyde (OPA) and 2-mercaptoacetic acid was developed for the determination of apramycin, an aminoglycoside antibiotic used in veterinary medicine, in the oral soluble powder form. The chromatographic separation was done by ion-pair HPLC using a C18 reversed-phase column, Synergy Hydro (150 mm x 4.6 mm x 4 µm) and mobile phase composed of 0.005 mol/L sodium octanosulfonate in a mixture of acetonitrile: water: acetic acid (45:55:2) (v/v/v) with a flow rate of 1.0 mL/min; the UV detector was operated at 332 nm. The developed method was validated according to official compendia guidelines, having demonstrated robustness, selectivity and linearity for the concentration range of 0.02 to 0.05 mg/mL, precision (with RSD < 2.0% both for intra and inter-day precision) accuracy (average recuperation of 99.33%) and detectivity (quantification and detection limits of 0.08 and 0.02 µg/mL, respectively). Three batches of commercial apramycin oral soluble powder were analyzed by both the proposed method and the official microbiological method, where all the results obtained were in the acceptable range (95% to 105% of labeled value of apramycin). Both methods were statistically compared by the t test, which yielded no significant differences (α = 0.05) thereby confirming the equivalence of the methods.


2007 ◽  
Vol 72 (1) ◽  
pp. 37-44 ◽  
Author(s):  
Jelena Stojanovic ◽  
Sote Vladimirov ◽  
Valentina Marinkovic ◽  
Dragan Velickovic ◽  
Predrag Sibinovic

A sensitive, selective, precise and stability-indicating, new high-performance liquid chromatographic method for the analysis of carvedilol both as a bulk drug and in formulations was developed and validated. As the method could effectively separate the drug from its degradation products, it can be employed as a stability-indicating one. The method was validated for linearity, selectivity, precision, robustness, LOD, LOQ and accuracy. The chromatographic separation was achieved on a Chromolit RP8e, 100x4.6 mm, analytical column. The mobile phase consisted of a mixture of acetonitrile and water (45:55, V/V) (pH 2.5), pH adjusted with formic acid. The absorbance was monitored with a UV detector at 280 nm and the temperature of the analyses was 40?C. The flow rate was 0.5 mL/min. The linearity (r? 0.999), reproducibility (0.68-1.27 %) and recovery (99.71-101.58) were found to be satisfactory. This method enables the simultaneous determination of carvedilol and its degradation products, as well as stability. .


2013 ◽  
Vol 2013 ◽  
pp. 1-4
Author(s):  
Suying Ma ◽  
Haixia Lv ◽  
Xiaojun Shang

A high performance liquid chromatographic (HPLC) method with UV detector for the determination of dyclonine hydrochloride and a gas chromatography (GC) method with flame ionization detector (FID) for the determination of camphor and menthol in lotion were developed. The developed HPLC method involved using a SinoChoom ODS-BP C18reversed-phase column (5 μm, 4.6 mm × 200 mm) and mobile phase consisting of acetonitrile : water : triethylamine in a ratio of 45 : 55 : 1.0; pH was adjusted to 3.5 with glacial acetic acid. The developed GC method for determination of camphor and menthol involved using an Agilent 19091J-413 capillary chromatographic column (30 m × 320 μm × 0.25 μm). The two methods were validated according to official compendia guidelines. The calibration of dyclonine hydrochloride for HPLC method was linear over the range of 20–200 μg/mL. The retention time was found at 6.0 min for dyclonine hydrochloride. The calibration of camphor and menthol of GC method was linear over the range of 10–2000 μg/mL. The retention time was found at 2.9 min for camphor and 3.05 min for menthol. The proposed HPLC and GC methods were proved to be suitable for the determination of dyclonine hydrochloride, camphor, and menthol in lotion.


INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (07) ◽  
pp. 43-49
Author(s):  
B.P. Manjula ◽  
V. G Joshi ◽  
Siddamsetty Ramachandra Setty ◽  
M Geetha ◽  

Tea tree oil, an active ingredient of skin, hair and nail care cosmeceuticals, has claims for topical antimicrobial, analgesic and anti-inflammatory activity. Its complex composition is governed by ISO 4730:2017. Terpinene-4-ol is the principal constituent of the oil (35% - 48%) followed by γ-terpinene (14% -28%), α-terpinene (6%-12%) and 1,8-cineole (≤15%). A reversed-phase, isocratic high performance liquid chromatographic method has been developed and validated for routine determination of tea tree oil based on1,8-cineole content in bulk and commercially available cosmeceuticals using C18 column, methanol-water (70:30 v/v) as mobile phase and flow rate of 1mL/min. UV detection was done at 200 nm. Linearity of the method was established for 20-100μL/mL (R2 = 0.9992) with LOD, LOQ values of 0.5594 μL/mL and 5.5941μL/mL respectively. The % RSD values for robustness and precision were <1% and recovery ranged between 99.09-102.96%. The method was successfully applied for determination of 1,8-cineole content in cosmeceuticals.


Author(s):  
M. Murali ◽  
P. Venkateswara Rao

A simple, selective, linear, precise and accurate isocratic RP-HPLC method was developed and validated for rapid assay of Vandetanib, an anticancer drug, in both bulk and tablet dosage form. Elution at a flow rate of 1ml/min was employed on a symmetry C18 column at ambient temperature. The mobile phase consisted of acetonitrile, water and orthophosphoric acid in the ratio of 90:08:02 (v/v/v). Linearity was observed in concentration range of 50-200 ppm. The retention time for Vandetanib was 3.326 min. The method was validated as per the ICH guidelines. The proposed method can be successfully applied for the estimation of Vandetanib in pharmaceutical dosage forms. Moreover the detection alone was also verified through LC-MS of the Vandetanib drug using ESI method which provides future scope for study of this drug using LC-MS method also.


Author(s):  
Zahid Zaheer ◽  
Sarfaraz Khan ◽  
Mohammad Sadeque ◽  
Hundekari G. I. ◽  
Rana Zainuddin

A simple, reproducible and efficient reverse phase high performance liquid chromatographic method was developed for Lisinopril in bulk drug and formulation. A column having 150 × 4.6 mm in isocratic mode with mobile phase containing acetonitrile: phosphate buffer (70:30; adjusted to pH 3.0) was used. The flow rate was 0.8 ml/min and effluent was monitored at 216 nm. The retention time (min) and linearity range (μg/ml) for Lisinopril was (1.510) and (10-35). The developed method was found to be accurate, precise and selective for determination of Lisinopril in bulk and formulation.


2017 ◽  
Vol 1 (2) ◽  
pp. 1-8
Author(s):  
Milena Cristina Ribeiro Souza Magalhães ◽  
Alisson Samuel Portes Caldeira ◽  
Hanna De Sousa Rocha Almeida ◽  
Sílvia Ligório Fialho ◽  
Armando Da Silva Cunha Junior

A reversed-phase high-performance liquid chromatographic (HPLC) method was developed and validated for the determination of encapsulation efficiency of zidovudine in nanoparticules. The method was carried out in isocratic mode using 0.040M sodium acetate: methanol: acetonitrile: glacial acetic acid (880:100:20:2) as mobile phase, a C8 column at 25ºC and UV detection at 240 nm. The method was linear (r2 ˃ 0.99) over the range of 25.0-150.0 μg/mL, precise (RSD ˂ 5%), accurate (recovery = 100.5%), robust and selective. The validated HPLC-UV method can be successfully applied to determine the rate of zidovudine in nanoparticules.


Author(s):  
Abrar Ahmed ◽  
Tayyaba Mahtab ◽  
Sumaiyya Saleem

Midostaurin is a multi-targeted protein kinase inhibitor that has been used for the treatment of acute myeloid leukemia.  Here, a rapid and precise reverse phase high-performance liquid chromatographic method has been developed for the validation of midostaurin, in its API form as well as in capsule dosage form. Chromatography was carried out on a X-Bridge C18 (4.6 x 250 mm, 5 µm) column using a mixture of methanol: water (75:25% v/v) as the mobile phase at a flow rate of 1.0 mL/min, the detection was carried out at 243nm and the retention time of the midostaurin was found to be 3.155. The method produce linear responses in the concentration range of 10-50 µg/mL of midostaurin. The method precision for the determination of assay was below 2.0 % RSD. The LOD and LOQ values obtained were 1.2 µg/mL and 3.8 µg/mL respectively. There were no significant changes observed upon changing chromatographic conditions indicating the method to be robust. Therefore this validated method can be useful in the quality control of bulk and pharmaceutical formulations of midostaurin. 


2013 ◽  
Vol 49 (3) ◽  
pp. 521-528 ◽  
Author(s):  
Viviane Benevenuti Silva ◽  
Angel Arturo Gaona Galdos ◽  
Cintia Maria Alves Mothe ◽  
Michele Bacchi Pallastrelli ◽  
Maria Segunda Aurora Prado ◽  
...  

A simple, rapid, economical and reliable high performance liquid chromatographic method has been developed and successfully applied in simultaneous determination of ethinyl estradiol and drospirenone in coated tablets. The HPLC method was performed on a LiChroCART® 100RP column (125x4 mm i.d., 5 µm) with acetonitrile:water 50:50 (v/v) as mobile phase, pumped at a flow rate of 1.0 mL.min-1. The fluorescence detection for ethinyl estradiol was made at λex= 280 nm and λem= 310 nm and a UV detection for drospirenone was made at 200 nm. The elution time for ethinyl estradiol and drospirenone were 4.0 and 5.7 min, respectively. The method was validated in accordance to USP 34 guidelines. The proposed HPLC method presented advantages over reported methods and is suitable for quality control assays of ethinyl estradiol and drospirenone in coated tablets.


2008 ◽  
Vol 73 (6) ◽  
pp. 665-671 ◽  
Author(s):  
Snezana Mitic ◽  
Gordana Miletic ◽  
Danijela Kostic ◽  
Daniela Naskovic-Ðokic ◽  
Biljana Arsic ◽  
...  

An accurate, sensitive and reproducible high performance liquid chromatographic (HPLC) method for the quantification of doxycycline hyclate in pharmaceutical samples has been developed and validated. The drug and the standard were eluted from a Lichrosorb RP-8 (250 mm x 4.6 mm, 10 mm particle size) at 20?C with a mobile phase consisting of methanol, acetonitrile and 0.010 M aqueous solution of oxalic acid (2:3:5, v/v/v). The flow rate was 1.25 ml min-1. A UV detector set at 350 nm was used to monitor the effluent. Each analysis required no longer than 4 min. The limits of detection and quantification were 1.15 and 3.84 ?g ml-1, respectively. Recoveries for different concentrations ranged from 99.58 to 101.93%.


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