Determination of Neostigmine Bromide by Ion-Pairing Column Chromatography

1973 ◽  
Vol 56 (1) ◽  
pp. 128-131
Author(s):  
Rita E Kling
Keyword(s):  
Standard Deviation ◽  
Hydrolysis Product ◽  
Ion Pairing ◽  
Commercial Products ◽  
Product Standard ◽  
Ophthalmic Solutions ◽  
Column Chromatographic ◽  
Sensitive Method ◽  
Good Agreement

Abstract A rapid and sensitive method for the assay of neostigmine bromide (NBr) in tablets and ophthalmic solutions has been developed. NBr is isolated from its pharmaceutical excipients by the ion-pairing partition column chromatographic principles of Levine and Doyle followed by ultraviolet determination of its alkaline hydrolysis product. Standard recoveries of NBr from simulated tablet mixtures and ophthalmic solutions averaged 99.8%. The standard deviation of repeated analyses of commercial products was less than±1%. The results of the proposed method for commercial products are in good agreement with the USP XVIII procedure. The procedure is applicable to individual tablet assay.

Collaborative Study of Ion-Pairing Column Chromatographic Determination of Neostigmine Bromide

1974 ◽  
Vol 57 (3) ◽  
pp. 725-727
Author(s):  
Rita E Kling
Keyword(s):  
Collaborative Study ◽  
Ophthalmic Solution ◽  
Ion Pairing ◽  
Chromatographic Determination ◽  
Relative Standard ◽  
The Individual ◽  
Tablet Preparation ◽  
Ophthalmic Solutions ◽  
Column Chromatographic

Abstract A revised version of the ion-pairing column chromatographic method for neostigmine bromide in tablets and ophthalmic solutions was subjected to a collaborative study. Eleven collaborators assayed a commercial tablet preparation, a simulated tablet formulation, 5 individual tablets, and a simulated ophthalmic formulation. The relative standard deviations were 2.2, 1.8, and 1.5% for the 2 tablet samples and the ophthalmic solution, respectively, and 2.4% for the individual analysis. The method has been adopted as official first action.

Automated Method for the Analysis of Riboflavin in Milk, with Application to Other Selected Foods

1974 ◽  
Vol 57 (5) ◽  
pp. 1085-1088
Author(s):  
James R Kirk
Keyword(s):  
Standard Deviation ◽  
Continuous Flow ◽  
Quantitative Method ◽  
Green Fluorescence ◽  
Internal Standards ◽  
Automated Method ◽  
Sodium Hydrosulfite ◽  
Automated Technique ◽  
Good Agreement

Abstract A continuous flow automated technique was developed for the determination of riboflavin in milk. The determination is based on the measurement of the natural yellow-green fluorescence of riboflavin at an excitation of 436 nm and emission of 510 nm. Blank values are determined for each sample after sodium hydrosulfite reduction of the riboflavin. Mean recovery and standard deviation for riboflavin in milk determined by the continuous flow procedure using internal standards were 9 7% and ± 2.42%, respectively. The recovery value was in good agreement with that determined using a manual procedure, while the standard deviation was 33% less than that found when using the manual procedure. The results from this study indicate that the continuous flow automated procedure for the determination of riboflavin in milk is a simple, quantitative method which eliminates many of the time-consuming analytical steps.

scholarly journals Flotation-Spectrophotometric Method for the Determination of Aluminium ion Using Xylenol Orange

2011 ◽  
Vol 8 (4) ◽  
pp. 1528-1535 ◽  
Author(s):  
F. Nekouei ◽  
Sh. Nekouei
Keyword(s):  
Standard Deviation ◽  
Spectrophotometric Method ◽  
Calibration Curve ◽  
Limit Of Detection ◽  
Xylenol Orange ◽  
Molar Absorptivity ◽  
Relative Standard ◽  
Ion Associate ◽  
Sensitive Method

A simple, fast, reproducible and sensitive method for the flotation- spectrophotometric determination of Al3+is reported. The apparent molar absorptivity (ε) of the ion associate was determined to be 8.35×104L mol-1cm-1. The calibration curve was linear in the concentration range of 1.0-50 ng mL-1of Al3+with a correlation coefficient of 0.9997. The limit of detection (LOD) was 0.621 ng mL. The relative standard deviation (RSD) at 10 and 30 ng mL-1of aluminium were 1.580 and 2.410% (n=7) respectively. The method was applied for measuring the amount of aluminium in water samples.

SIMS Determination of MG+ and AS+ Range Profiles in Photoresist and Polyimide Implant Masks.

1989 ◽  
Vol 147 ◽  
Author(s):  
D. L. Dugger ◽  
M. B. Stern ◽  
T. M. Rubico
Keyword(s):  
Standard Deviation ◽  
Mass Spectroscopy ◽  
Range Data ◽  
Profile Data ◽  
Projected Range ◽  
Range Profile ◽  
P Type ◽  
Secondary Ion ◽  
Good Agreement

AbstractThe distribution of Mg+ (a p-type dopant for GaAs) and As+ (an p-type dopant for Si) implanted into both photoresist (PR) and polyimide (PI) have been determined experimentally. Range data of Mg ions at 200 keV and 300 keV and As ions at 150 keV have been measured by Secondary Ion Mass Spectroscopy (SIMS). SIMS values for the projected range Rp and the standard deviation ARp were compared to range profile data calculated using the Projected Range Algorithm (PRAL) of Biersack [1] as well as the standard LSS theory [2]. While the values for Rp calculated from the PRAL model generally agreed within 10% of the SIMS values, the calculations underestimated Rp for PR but were in good agreement for PI. The LSS calculations underestimated Rp in both materials.

Determination of Cephapirin and Desacetylcephapirin in Milk Using Automated Liquid Chromatographic Cleanup and Ion-Pairing Liquid Chromatography

1993 ◽  
Vol 76 (3) ◽  
pp. 535-540 ◽  
Author(s):  
William A Moats
Keyword(s):  
Liquid Chromatography ◽  
Detection Limits ◽  
Ion Pairing ◽  
Screening Tests ◽  
Tetraethylammonium Chloride ◽  
Liquid Chromatographic ◽  
Sensitive Method

Abstract A simple and sensitive method was developed for determination of cephapirin and its metabolite, desacetylcephapirin, in milk. For extraction/ deproteinization, 2 mL 0.2M tetraethylammonium chloride and 28 mL acetonitrile are added to 10 mL milk, and 20 mL clear filtrate (= 5 mL milk) is collected. Filtrate is evaporated to 1-2 mL and made up to 4 mL with water, filtered, and transferred to 4 mL autosampler vials. For cleanup, 2 mL filtrate is loaded onto a Supelcosil LC-18 column in 0.01 M KH2PO4 (A) using a Waters WISP autosampler. The column is eluted with an acetonitrile (B) gradient from 100%A (0-3 min) to 70%A:30%B (24 min). Fractions corresponding to cephapirin and desacetylcephapirin are collected. A 0.02M pH 2.26 buffer of 0.01 M decanesulfonate-acetonitrile was used for cephapirin (80 + 20) and 0.02M pH 1.96 buffer of 0.01 M decanesulfonate-acetonitrile was used for desacetylcephapirin (84 + 16) on a Polymer Laboratories PLRP-S column. Recoveries at 0.01-10 ppm were 91-98%; estimated detection limits were near 2 ppb and were comparable to sensitive screening tests.

Amino Acid Analysis in Feeds and Feedstuifs Using Precolumn Phenylisothiocyanate Derivatization and Liquid Chromatography—Preliminary Study

1987 ◽  
Vol 70 (3) ◽  
pp. 425-428 ◽  
Author(s):  
Rodney W Beaver ◽  
David M Wilson ◽  
Helen M Jones ◽  
Keith D Haydon
Keyword(s):  
Amino Acids ◽  
Liquid Chromatography ◽  
Standard Deviation ◽  
Poultry Feed ◽  
Reverse Phase ◽  
Relative Standard ◽  
Preliminary Study ◽  
Feed Samples ◽  
Good Agreement

Abstract A method for the determination of amino acids in feed hydrolysates is described. The method uses precolumn phenylisothiocyanate (PITC) derealization and liquid chromatography on reverse phase columns with UV detection at 254 nm. The precision of the method on replicate samples of a wheat hydrolysate ranges from 1.9 to 6.7% relative standard deviation for the amino acids examined. (Met and Cys were not determined.) Recoveries were near 100% for most amino acids. Comparisons of the values obtained by PITC method with accepted wines show good agreement in wheat and poultry feed samples.

THE USE OF FURFURAL FOR THE DETERMINATION OF ACETONE BODIES IN BIOLOGICAL FLUIDS

1958 ◽  
Vol 36 (1) ◽  
pp. 1047-1056 ◽  
Author(s):  
John B. Lyon Jr. ◽  
Walter L. Bloom
Keyword(s):  
Standard Deviation ◽  
Biological Fluids ◽  
Strong Acid ◽  
Water Bath ◽  
Effective Range ◽  
Average Standard Deviation ◽  
Strong Base ◽  
Violet Color ◽  
Sensitive Method

A rapid and sensitive method for the determination of acetone plus acetoacetate, and total acetone bodies in blood and urine is described. It is based upon the condensation of acetone and furfural in the presence of a strong base to form difurfurylidene–acetone, which develops a red to violet color in strong acid. A standard Thunberg tube, which is heated and cooled in a water bath, is used as a microrefluxing and a microdistillation unit. The effective range is from 1 to 6 μg of acetone per sample. The average standard deviation, based on recoveries of added material, was 5%. When the method was applied to determinations of blood and urine of several species, the results agreed with those reported by others.

THE USE OF FURFURAL FOR THE DETERMINATION OF ACETONE BODIES IN BIOLOGICAL FLUIDS

1958 ◽  
Vol 36 (10) ◽  
pp. 1047-1056 ◽  
Author(s):  
John B. Lyon Jr. ◽  
Walter L. Bloom
Keyword(s):  
Standard Deviation ◽  
Biological Fluids ◽  
Strong Acid ◽  
Water Bath ◽  
Effective Range ◽  
Average Standard Deviation ◽  
Strong Base ◽  
Violet Color ◽  
Sensitive Method

A rapid and sensitive method for the determination of acetone plus acetoacetate, and total acetone bodies in blood and urine is described. It is based upon the condensation of acetone and furfural in the presence of a strong base to form difurfurylidene–acetone, which develops a red to violet color in strong acid. A standard Thunberg tube, which is heated and cooled in a water bath, is used as a microrefluxing and a microdistillation unit. The effective range is from 1 to 6 μg of acetone per sample. The average standard deviation, based on recoveries of added material, was 5%. When the method was applied to determinations of blood and urine of several species, the results agreed with those reported by others.

Kinetic Spectrophotometric Determination of Selenium (IV) by its Catalytic Effect on the Oxidation of Acid Chrome Blue K by Hydrogen Peroxide

2012 ◽  
Vol 538-541 ◽  
pp. 2358-2363 ◽  
Author(s):  
Zhi Rong Zhou ◽  
Li Zhen Zhang
Keyword(s):  
Hydrogen Peroxide ◽  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Limit Of Detection ◽  
Fixed Time ◽  
Relative Standard ◽  
Kinetic Spectrophotometric ◽  
Acid Chrome Blue K ◽  
Good Agreement

Based on the oxidation of acid chrome blue K (ACBK) by hydrogen peroxide in 0.002 mol/L sulfuric acid solution, while 1,10-phenanthroline (phen) acts as an activator, a simple kinetic spectrophotometric method was developed for the determination of trace amounts of Se(IV).The reaction was monitored spectrophotometrically by measuring the decrease in the absorbance of ACBK at 524 nm with a fixed-time method. The decrease in the absorbance of ACBK is proportional to the concentration of Se (IV) in the range 0.06–1.0 µg/L with a fixed time of 4–10 min from the initiation of the reaction. The limit of detection is 0.018 µg/L Se (IV). The influence of the factors such as acidity, concentration of reactants, reaction time, temperature and co-existing ions on the reaction is discussed. The optimum conditions of reaction are established and some kinetic parameters are determined. The apparent activation energy of catalytic reaction is 62.30 kJ/mol. The relative standard deviation for 11 replicate determination of 0.01 and 0.02 µg/25mL selenium (III) was calculated to be 2.3 % and 2.0 %, respectively. Combined with sulphydryl dextrane gel (SDG) separation and enriching, the method has been successfully applied to the determination of Se (IV) in foodstuff samples with the relative standard deviation of 1.1 %–3.7 % and the recovery of 99.0 %–104.0 %, the results are in good agreement with those provided by HG-AAS method.

Automated Fluorometric Method For The Determination of Serum Calcium

1969 ◽  
Vol 15 (9) ◽  
pp. 870-878 ◽  
Author(s):  
Benjamin Fingerhut ◽  
Alfred Poock ◽  
Henry Miller
Keyword(s):  
Standard Deviation ◽  
Serum Calcium ◽  
Fluorometric Method ◽  
Good Agreement

Abstract An automated fluorometric procedure for serum calcium has been developed which can be used for a wider variety of pathologic serums than the automated fluorometric and colorimetric technics generally being used at present. The method is based upon measurement of the fluorescence produced by calcein with calcium in a serum dialysate. Results are in good agreement with the Clark-Collip procedure. Recovery experiments averaged 98-101%. The standard deviation for duplicate determinations averaged ±0.20 mg/100 ml.

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