High Performance Liquid Chromatographic Determination of Furazolidone in Feed and Feed Premixes

1981 ◽  
Vol 64 (5) ◽  
pp. 1100-1104
Author(s):  
Robert L Smallidge ◽  
Norman W Rowe ◽  
Nandan D Wadgaonkar ◽  
Rodger W Stringham
Keyword(s):  
Standard Deviation ◽  
Relative Standard Deviation ◽  
High Performance ◽  
Colorimetric Assay ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Tetraethylammonium Bromide ◽  
Precision Data ◽  
Relative Standard ◽  
Field Samples

Abstract Furazolidone is separated from finished feeds by acetone-water extraction on a Goldfisch apparatus. Extracting solvent is removed, and the residue is dissolved in dimethylformamide-5% tetraethylammonium bromide (1 + 1), clarified, and chromatographed on a reverse phase C18 column. The mobile phase is CH3CN-2% acetic acid (20 + 80) with detection at 365 nm. The method was tested for linearity, recovery, and ruggedness, and compared with the AOAC colorimetric assay by using field samples containing 0.0055-0.055% furazolidone. Precision data suggest a cumulative relative standard deviation of 1.43% within days and 1.78% between days. The ruggedness test predicts a between-laboratory relative standard deviation of 3.67%. Recovery was 97.5 ± 2.0% and linearity was excellent (r2 = 0.9994) up to 0.06% furazolidone. Premixes are extracted by shaking with dimethylformamide. An aliquot of the extract is diluted (1 + 1) with 5% tetraethylammonium bromide, clarified, and chromatographed.

scholarly journals Liquid Chromatographic Determination of Deoxynivalenol in Baby Food and Animal Feed: Interlaboratory Study

2006 ◽  
Vol 89 (4) ◽  
pp. 1012-1020 ◽  
Author(s):  
Joerg Stroka ◽  
Michelle Derbyshire ◽  
Carsten Mischke ◽  
Massimo Ambrosio ◽  
Katy Kroeger ◽  
...  
Keyword(s):  
Standard Deviation ◽  
Relative Standard Deviation ◽  
High Performance ◽  
Animal Feed ◽  
Chromatographic Determination ◽  
Baby Food ◽  
Interlaboratory Study ◽  
Relative Standard ◽  
Liquid Chromatographic

Abstract An interlaboratory study was conducted for the determination of deoxynivalenol in baby food and animal feed by high-performance liquid chromatography with UV detection. The study included 14 participants representing a cross section of industry, official food control, and research facilities. Mean recoveries reported ranged from 89% (at 120 g/kg) to 85% (at 240 g/kg) for baby food and from 100% (at 200 g/kg) to 93% (at 400 g/kg) for animal feed. On the basis of the results for spiked samples (blind duplicates at 2 levels), as well as those for naturally contaminated samples (blind duplicates at 3 levels), the relative standard deviation for repeatability (RSDr) in analyses of baby food ranged from 6.4 to 14.0% and in analyses of animal feed, from 6.1 to 16.5%. The relative standard deviation for reproducibility (RSDR) in analyses of baby food ranged from 9.4 to 19.5% and in analyses of animal feed, from 10.5 to 25.2%. The HorRat values ranged from 0.4 to 1.0 and from 0.7 to 1.3, for baby food and animal feed, respectively. The method showed acceptable performance for within-laboratory and between-laboratory precision for each matrix, as required by European legislation.

scholarly journals Validation of a high-performance liquid chromatographic method with fluorecence detection for the quantification of flurbiprofen in tablets

2018 ◽  
Vol 34 (2) ◽  
Author(s):  
Thi Thanh Binh Nguyen ◽  
Anh Mai Tran ◽  
Thuan Hai Duong ◽  
Tung Huu Nguyen ◽  
Tung Thanh Bui
Keyword(s):  
Standard Deviation ◽  
Relative Standard Deviation ◽  
High Performance ◽  
Chromatographic Method ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Intermediate Precision ◽  
Liquid Chromatographic Method ◽  
Relative Standard ◽  
Liquid Chromatographic

In this study, a high-performance liquid chromatographic method with fluorecence detection was developed for the quantification of flurbiprofen in tablets. A C8 reverse phase column (5 μm, 120 Å, 4.6×150 mm) was used with a mobile phase of acetonitrile : water : glacial acetic acid (65 : 32.5 : 2.5, v/v/v) . The flow rate was 1 ml/min and the column effluent was monitored within 8 minutes. The excitation and emission wavelength were respectively 247 nm and 312 nm. The temperature of flow cell was set at 45˚C and detector sensitivity was 5. The retention time of flurbiprofen was found to be 3.78 minutes. The method was validated under the concentration range of 5 - 100 ng/ml with a tight linear correlation between peak area and sample concentration (R = 0.9999). The proposed method was found to be specific to flurbiprofen, accurate and precise. The percentage recovery was ≤ 100 ± 2%, the relative standard deviation of the repeatability was ≤ 2.08% and the relative standard deviation of the intermediate precision was ≤ 2.96%. The limit of detection and limite of quantification were respectively 0.010 and 0.025 ng/ml.

scholarly journals Assay method development and validation for butamben drug substance by using high performance liquid chromatographic technique

2020 ◽  
Vol 11 (1) ◽  
pp. 981-984
Author(s):  
Sachin D. Zade ◽  
Padma S. There ◽  
Sunanda S. Aswale ◽  
Shashikant R. Aswale
Keyword(s):  
Standard Deviation ◽  
Relative Standard Deviation ◽  
High Performance ◽  
Method Development ◽  
High Performance Liquid Chromatographic ◽  
Drug Substance ◽  
Assay Method ◽  
Forced Degradation ◽  
Chromatographic Technique ◽  
Relative Standard

Stability indicating assay methodology was developed with UV detection for the simultaneous quantification of Butamben drug substance by HPLC. The separation between degradation impurities and the peak due to Butamben was achieved by using Universal C 18, (100 x 4.6) mm, 5.0-micron column. Mobile Phase was made up of Water, Methanol and Orthrophosphoric acid by mixing 350:650:1 ml, respectively. Isocratic method was used by using flow rate of 1.0 ml/min, UV at 250 nm and column oven temperature at 50°C. Relative standard deviation for standard preparation under system precision was achieved within acceptance criteria. Relative standard deviation for retention time was achieved 0.11%, which shows reproducibility during replicate injections. After the successful development of this method, chemically forced degradation was performed by external acid, alkali and peroxide treatment. Not any degradation peak was interfering with any impurity. This newly developed innovative method is found suitable for the Assay analysis of Butamben API.

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 Determination of Neutral Lactase Activity in Industrial Enzyme Preparations by a Colorimetric Enzymatic Method: Collaborative Study

1999 ◽  
Vol 82 (1) ◽  
pp. 112-118 ◽  
Author(s):  
Adrianus J Engelen ◽  
Peter H G Randsdorp ◽  
R Cassaigne ◽  
S M Dutta ◽  
M Harboe ◽  
...  
Keyword(s):  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Colorimetric Assay ◽  
Collaborative Study ◽  
Enzymatic Method ◽  
Lactase Activity ◽  
Method Performance ◽  
Enzyme Preparations ◽  
Industrial Enzyme ◽  
Relative Standard

Abstract Thirteen laboratories participated in a collaborative study to validate a colorimetric assay for determining neutral lactase activity in industrial enzyme preparations. Each laboratory received 5 duplicate samples with activity levels of 2000 and 5000 neutral lactase units provided by 4 commercial suppliers. Two laboratories did not return results. Method performance was calculated according to AOAC guidelines. From the 11 remaining laboratories, 3 were excluded from statistical analysis because of invalid data determined during initial review by Youden pair, value versus laboratory. Repeatability relative standard deviation (RSDr) values ranged from 3.20 to 8.62%, and reproducibility relative standard deviation (RSDR) values ranged from 8.77 to 16.35%. With outliers excluded, RSDr values ranged from 2.94 to 5.01%, and RSDRvalues ranged from 7.50 to 13.84%. The colorimetric enzymatic method for determining neutral lactase activity in industrial enzyme preparations has been adopted first action by AOAC INTERNATIONAL.

High Performance Liquid Chromatographic Determination of Primidone in Tablets

1982 ◽  
Vol 65 (5) ◽  
pp. 1063-1065
Author(s):  
Stanley E Roberts
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Average Recovery ◽  
Relative Standard ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A high performance liquid chromatographic (HPLC) method is described for the quantitative determination of primidone in tablets. A ground tablet sample is diluted directly in the mobile phase, at a concentration of about 1 mg/mL of primidone, mixed and deaerated, and filtered. The resulting solution is then quantitated by HPLC. The average spike recoveries for the 50 mg and 250 mg tablets were 101.2% and 99.0%, respectively. The average recovery for an authentic mixture formulated at the 250 mg level was 100.1% with a relative standard deviation of 0.45%.

Liquid Chromatographic Determination of Narasin in Feed Premixes

1985 ◽  
Vol 68 (3) ◽  
pp. 417-418 ◽  
Author(s):  
Raymond L Hussey ◽  
Thomas D Macy ◽  
John Moran ◽  
Andrew Loh
Keyword(s):  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Chromatographic Determination ◽  
Bioassay Method ◽  
Water Solvent ◽  
Relative Standard ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A liquid chromatographic (LC) method has been developed to determine narasin in feed premixes. Narasin is extracted from the premix with a methanol-water solvent, and the extracted solution is assayed by using LC. Recovery of narasin from a 12.5 g/lb premix is quantitative (100%), with a relative standard deviation of 1.44%. The results correlated well (coefficient 0.92) with a turbimetric bioassay method.

scholarly journals Column High-Performance Liquid Chromatographic Determination of Norfloxacin and Its Main Impurities in Pharmaceuticals

2008 ◽  
Vol 91 (2) ◽  
pp. 332-338 ◽  
Author(s):  
Branislava Mielji ◽  
Gordana Popovi ◽  
Danica Agbaba ◽  
Slavko Markovi ◽  
Breda Simonovska ◽  
...  
Keyword(s):  
High Performance ◽  
Raw Materials ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Array Detector ◽  
Chromatographic Separations ◽  
Experimental Conditions ◽  
Relative Standard ◽  
Liquid Chromatographic

Abstract A gradient reversed-phase column high-performance liquid chromatographic method was developed for the detection and quantification of norfloxacin and its major impurities in norfloxacin-containing pharmaceuticals. Chromatographic separations were performed under the following experimental conditions: column, Zorbax SB RP-18 (5 m, 250 4.6 mm); injection volume, 20 L; mobile phase, 0.05 M NaH2PO4 (pH 2.5)acetonitrile (87 + 13) for 16 min and (58 + 42) for 9 min (stepwise gradient); and flow rate, 1.3 mL/min. All analyses were performed at 25C, and the eluate was monitored at 275 nm using a diode array detector. Linearity (correlation coefficient = 0.999), recovery (99.3101.8), relative standard deviation (0.20.7), and quantitation limit (0.120.47 g/mL) were evaluated and found to be satisfactory. The method is simple, rapid, and convenient for purity control of norfloxacin in both raw materials and dosage forms.

scholarly journals Immunoaffinity Column Cleanup with Liquid Chromatography for Determination of Aflatoxin M1 in Liquid Milk: Collaborative Study

2001 ◽  
Vol 84 (2) ◽  
pp. 437-443 ◽  
Author(s):  
Sylviane Dragacci ◽  
Frederic Grosso ◽  
John Gilbert ◽  
M Agnedal ◽  
L Hyndrick ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Collaborative Study ◽  
Aflatoxin M1 ◽  
Immunoaffinity Column ◽  
Precision Data ◽  
Relative Standard ◽  
Liquid Milk

Abstract A collaborative study was conducted to evaluate the effectiveness of an immunoaffinity column cleanup liquid chromatographic method for determination of aflatoxin M1 in milk at proposed European regulatory limits. The test portion of liquid milk was centrifuged, filtered, and applied to an immunoaffinity column. The column was washed with water, and aflatoxin was eluted with pure acetonitrile. Aflatoxin M1 was separated by reversed-phase liquid chromatography (LC) with fluorescence detection. Frozen liquid milk samples both naturally contaminated with aflatoxin M1 and blank samples for spiking, were sent to 12 collaborators in 12 different European countries. Test portions of samples were spiked at 0.05 ng aflatoxin M1 per mL. After removal of 2 noncompliant sets of results, the mean recovery of aflatoxin M1 was 74%. Based on results for spiked samples (blind pairs at 1 level) and naturally contaminated samples (blind pairs at 3 levels) the relative standard deviation for repeatability (RSDr) ranged from 8 to 18%. The relative standard deviation for reproducibility (RSDR) ranged from 21 to 31%. The method showed acceptable within- and between-laboratory precision data for liquid milk, as evidenced by HORRAT values at the low level of aflatoxin M1 contamination.

scholarly journals The Influence of a Humectant on the Retention by Humans of Solanesol from Cigarette Smoke (Part 2, Glycerin)

2009 ◽  
Vol 23 (6) ◽  
pp. 378-383
Author(s):  
SC Moldoveanu ◽  
WM III Coleman
Keyword(s):  
Standard Deviation ◽  
Cigarette Smoke ◽  
Relative Standard Deviation ◽  
Human Subject ◽  
High Performance ◽  
Sample Collection ◽  
Human Respiratory Tract ◽  
Hygroscopic Properties ◽  
Cigarette Butts ◽  
Relative Standard

AbstractTwo common humectants are used as additives in the cigarette manufacturing process, propylene glycol (PG) and glycerin. The humectants may influence the deposition of cigarette smoke in the human respiratory tract by affecting the hygroscopic properties and growth of smoke particles. This study examines the influence of glycerin addition on the retention of solanesol by smokers. The influence of PG addition has been previously reported (7). The first cigarette used in the study (control) was a commercially available brand containing no additives in the blend (with a measured level of glycerin of 0.19%). The other cigarette (test) had an identical tobacco blend to the control, but had 2.3% added glycerin. The construction of the cigarette with 2.3% glycerin (test) was selected to match as closely as possible the ‘tar’ (as measured by Federal Trade Commission regimen), pressure drop (open and closed), and nicotine level of the commercial cigarette (control). Twelve smokers evaluated both products. The sample collection was performed using three cigarettes smoked within one hour. Each human subject smoked the control cigarette and then the test cigarette in two separate sessions. The exhaled smoke was collected using a vacuum assisted procedure designed to avoid strain in exhaling, and solanesol was analyzed using an high performance liquid chromatography (HPLC) technique. The cigarette butts from the smokers were collected and also analyzed for solanesol. The results obtained for the cigarette butts from the smokers were used to calculate the level of solanesol in the smoke delivered to the human subject, based on calibration curves. These curves were generated separately by analyzing the solanesol in smoke and in the cigarette butts obtained by machine smoking under different puffing regimes. Knowing the levels of delivered amount of solanesol and that in the exhaled smoke it was possible to calculate the retention of this compound from mainstream smoke for the two cigarette types. The amount of solanesol retained by the smoker (per cigarette) was on average 314.8 µg/cig with 18.9% relative standard deviation for the commercial cigarette, and 302.6 µg/cig with 20.3% relative standard deviation for the cigarette with 2.3% added glycerin. The retention % of solanesol from the commercial cigarette showed an average of 69.5% with 9.4% relative standard deviation, and the cigarette with 2.3% added glycerin showed an average retention of 69.4% with 10.5% relative standard deviation. Applying the paired t-test to the data it was found that there were no significant differences in the retention amount of solanesol, or in the retention % of solanesol for the two cigarettes. No correlation was found between the amount of solanesol delivered to the smoker (in µg/cig) and the solanesol retention % by the smoker.

Sign in / Sign up

Export Citation Format

Share Document