Liquid Chromatographic Method for Determining the Percent of Olestra in Lipid Samples

1993 ◽  
Vol 76 (6) ◽  
pp. 1396-1399 ◽  
Author(s):  
Daniel H Tallmadge ◽  
Y T Lin Peter
Keyword(s):  
Soybean Oil ◽  
Cottonseed Oil ◽  
Reversed Phase ◽  
Evaporative Light Scattering Detector ◽  
Liquid Chromatographic Method ◽  
Evaporative Light Scattering ◽  
Lipid Sample ◽  
Liquid Chromatographic ◽  
Peak Retention Time ◽  
Reversed Phase Lc

Abstract A liquid chromatographic (LC) method has been developed to determine the percent of olestra in lipid samples. To achieve the highest degree of accuracy, this method requires the use of an olestra standard with the same molecular composition as the olestra in the lipid sample to be analyzed. Samples were analyzed by reversed-phase LC using an evaporative light-scattering detector. Chromatography was performed with a 5 μm octadecylsilane- Zorbax column that separates olestra from other lipophilic components. Three types of olestra standards (soybean-oil olestra, unheated cottonseed- oil olestra, and heated cottonseed-oil olestra), each analyzed in soybean oil, showed linearity when the amount of olestra injected ranged from 20 to 160 fig (r= 0.9996). The area under the olestra peak (retention time 3.5 to 4.9 min) was used to quantify the amount of olestra in olestra-lipid samples, by comparing the olestra area for the sample with that of the standard using a curve derived by linear regression. The method was evaluated using 3 types of olestra blended with soybean oil and varying the percent of olestra in the olestra-lipid blend from 5 to 90%. Recovery of olestra from these olestra-lipid blends varied from 99.2 to 106.0%, demonstrating excellent accuracy, with method precision expressed as the coefficient of variation, 0.9%. Each error estimate was derived from 5 parallel determinations. With proper validation (e.g., running an olestra-free blank for each lipid matrix), this method provides a rapid, accurate, and precise technique for measuring the percent of olestra in lipids extracted from olestra-formulated foods and in olestra-lipid blends.

scholarly journals Liquid Chromatographic Method for Determining the Concentration of Bisazir in Water

1997 ◽  
Vol 80 (5) ◽  
pp. 1111-1116 ◽  
Author(s):  
Ronald J Scholefield ◽  
Karen S Slaght ◽  
John L Allen
Keyword(s):  
Great Lakes ◽  
Solid Phase ◽  
Reversed Phase ◽  
Lake Huron ◽  
Extraction Column ◽  
Treated Effluent ◽  
Liquid Chromatographic Method ◽  
Sea Lampreys ◽  
Liquid Chromatographic ◽  
Reversed Phase Lc

Abstract Barrier dams, traps, and lampricides are the techniques currently used by the Great Lakes Fishery Commission to control sea lampreys {Petromyzon marinug) in the Great Lakes. To augment these control techniques, a sterile-male-release research program was initiated at the Lake Huron Biological Station. Male sea lampreys were sterilized by intraperitoneal injection of the chemical sterilant P,P-bis(1-aziridinyl)-Nmethylphosphinothioic amide (bisazir). An analytical method was needed to quantitate the concentration of bisazir in water and to routinely verify that bisazir (>25 μg/L) does not persist in the treated effluent discharged from the sterilization facility to Lake Huron. A rapid, accurate, and sensitive liquid chromatographic (LC) method was developed for determining bisazir in water. Bisazir was dissolved in Lake Huron water; extracted and concentrated on a C18 solid-phase extraction column; eluted with methanol; and quantitated by reversed-phase LC using a Cis column, amobile phase of 70% water and 30% methanol (v/v), and UV detection (205 nm). Bisazir retention time was 7-8 min; total run time was about 20 min. Method detection limit for bisazir dissolved in Lake Huron water was about 15 μg/L. Recovery from Lake Huron water fortified with bisazir at 100 μg/L was 94% (95% confidence interval, 90.2-98.2%).

Gradient Multipeak Liquid Chromatographic Method for Determination of Ardacin in Bulk Chemical and Premix Formulations

1995 ◽  
Vol 78 (2) ◽  
pp. 289-293
Author(s):  
Hafez Abdel-Kader ◽  
Myriam M Kobylkevich ◽  
Larry S Wigman ◽  
Govind K Menon
Keyword(s):  
Pilot Scale ◽  
Reversed Phase ◽  
Liquid Chromatographic Method ◽  
Relative Standard ◽  
External Standard ◽  
Bulk Chemical ◽  
Method Accuracy ◽  
Liquid Chromatographic ◽  
Reversed Phase Lc

Abstract A liquid chromatographic (LC) method was developed for the determination of ardacin in bulk chemical (78 to 100%, w/w anhydrous) and premix formulations (3.3 to 26.4%, w/w). The method is based on reversed-phase LC resolution of ardacin components and detection by UV absorbance at 220 nm. Ardacin has 10 components, and each component can be quantitated separately. Total ardacin is determined by summing the areas of the 10 component peaks. Calculations are performed using an external standard approach. The method is linear for ardacin at 50 to 150 μ/mL. The method accuracy for a typical bulk chemical is ± 1.5%, w/w (relative standard deviation [RSD], 1.6%), and recovery from a typical pilot scale premix is 99.9% (RSD, 3.4%). The method is useful for monitoring stability during storage.

Determination of Ardacin in Premix, Supplement, and Animal Feed by a Rapid and Sensitive Two-Peak Liquid Chromatographic Method with Correlation to a Gradient Multipeak Liquid Chromatographic Method

1994 ◽  
Vol 77 (6) ◽  
pp. 1341-1346
Author(s):  
Hafez Abdel-Kader ◽  
Sylvia V Fagan ◽  
Govtnd K Menon ◽  
Larry S Wigman ◽  
Frederic Chapin
Keyword(s):  
Chromatographic Method ◽  
Animal Feed ◽  
Reversed Phase ◽  
Protein Supplement ◽  
Cattle Feed ◽  
Liquid Chromatographic Method ◽  
Relative Standard ◽  
Liquid Chromatographic ◽  
Reversed Phase Lc

Abstract A rapid and sensitive 2-peak liquid chromatographic (LC) method is described for extracting and quantitating ardacin in premix, supplement, and animal feed formulations. Ardacin is extracted from the formulations and analyzed after dilution or cleanup by reversed-phase LC with UV detection at 220 nm. The method correlates well with a more information-rich gradient multipeak LC method. Recoveries for premix formulations ranged from 96.8% (relative standard deviation [RSD], 0.8%) to 103.7% (RSD, 1.3%) for laboratory samples spiked at levels ranging from 1.6 to 39.6% ardacin. Recoveries for protein supplement mash formulations ranged from 98.7% of claim (RSD, 4.1%) to 106.0% of claim (RSD, 7.7%) at ardacin levels ranging from 37.5 to 600 mg/lb. Recoveries for cattle feed ranged from 90.0% of claim (RSD, 11.9%) to 105.6% of claim (RSD, 2.7%) at ardacin levels ranging from 4 to 30 g/ton.

Development and Validation of Spectrophotometric and Liquid Chromatographic Methods for Estimation of Tigecycline in Injections

2020 ◽  
Vol 13 (5) ◽  
pp. 5148-5154
Author(s):  
Sagar Suman Panda ◽  
Ravi Kumar B.V.V.
Keyword(s):  
Area Under The Curve ◽  
Reversed Phase ◽  
Equal Concentration ◽  
Pharmaceutical Dosage Form ◽  
Liquid Chromatographic Method ◽  
Array Detection ◽  
The Difference ◽  
The One ◽  
Development And Validation ◽  
Liquid Chromatographic

Three new analytical methods were optimized and validated for the estimation of tigecycline (TGN) in its injection formulation. A difference UV spectroscopic, an area under the curve (AUC), and an ultrafast liquid chromatographic (UFLC) method were optimized for this purpose. The difference spectrophotometric method relied on the measurement of amplitude when equal concentration solutions of TGN in HCl are scanned against TGN in NaOH as reference. The measurements were done at 340 nm (maxima) and 410nm (minima). Further, the AUC under both the maxima and minima were measured at 335-345nm and 405-415nm, respectively. The liquid chromatographic method utilized a reversed-phase column (150mm×4.6mm, 5µm) with a mobile phase of methanol: 0.01M KH2PO4 buffer pH 3.5 (using orthophosphoric acid) in the ratio 80:20 %, v/v. The flow rate was 1.0ml/min, and diode array detection was done at 349nm. TGN eluted at 1.656min. All the methods were validated for linearity, precision, accuracy, stability, and robustness. The developed methods produced validation results within the satisfactory limits of ICH guidance. Further, these methods were applied to estimate the amount of TGN present in commercial lyophilized injection formulations, and the results were compared using the One-Way ANOVA test. Overall, the methods are rapid, simple, and reliable for routine quality control of TGN in the bulk and pharmaceutical dosage form. 

Sign in / Sign up

Export Citation Format

Share Document