High Performance Liquid Chromatographic Determination of Minor Saccharides in Corn Sugar: Collaborative Study

1982 ◽  
Vol 65 (6) ◽  
pp. 1366-1369
Author(s):  
C Earl Engel ◽  
Philip M Olinger ◽  
Raffaele Bernetti ◽  
◽  
K M Brobst ◽  
...  
Keyword(s):  
High Performance ◽  
Collaborative Study ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Liquid Chromatograph ◽  
Mean Values ◽  
Water Solvent ◽  
Coefficients Of Variation ◽  
Aoac Method

Abstract The official first action AOAC method for quantitative determination of saccharides in corn syrup by liquid chromatography was reinvestigated to expand its scope to products containing dextrose in excess of 98%. Because of the low levels of saccharides other than dextrose (DP1), separations are carried out only of the DP1, the disaccharides (DP2), and the tri- and higher saccharides (DP3+) on an Aminex Q15-S, calcium form, cation exchange column. Concentrations of solids in water solvent injected into the liquid chromatograph are higher than those in the AOAC method to increase precision of analysis of the minor saccharides. All carbohydrate components in solution are eluted from the column; therefore, loss of refractive index detector linearity with respect to dextrose is compensated by use of an external maltose (DP2) standard to correct for DP2 and DP3+ response and dextrose is calculated by difference from 100. With mean values of 0.520% DP2 and 0.244% DP3+, the reproducibility and repeatability coefficients of variation are 14.6 and 6.7% for DP2, and 19.3 and 11.9% for DP3+, respectively. Dextrose levels of 99.23% are reproducible within 0.161. The coefficients of variation of the DP2 component are lower by this method than by the AOAC method at levels up to 2% DP2. The method has been adopted official first action.

High Performance Liquid Chromatographic Determination of Carbaryl Insecticide in Formulations

1980 ◽  
Vol 63 (3) ◽  
pp. 650-652
Author(s):  
William H Mcdermott
Keyword(s):  
High Performance ◽  
Methylene Chloride ◽  
Collaborative Study ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Modified Silica Gel ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A high performance liquid chromatographic method for carbaryl in formulations has been developed and used to assay 3 formulations in a 10-day repeatability study. The method uses a cyano modified silica gel column packing and a mobile phase of heptane-methylene chloride-isopropanol-methanol (60+35+4.8+0.2). The coefficients of variation for 2 wettable powders and one aqueous flowable formulation were 0.61, 0.62, and 0.75%, respectively. It is recommended that a collaborative study be conducted on this method.

High Performance Liquid Chromatographic Determination of Methapyrilene Hydrochloride in Feed and Sleep Aid Tablets

1981 ◽  
Vol 64 (4) ◽  
pp. 889-892
Author(s):  
Badaruddin Shaikh ◽  
Margarette R Hallmark
Keyword(s):  
High Performance ◽  
Ammonium Carbonate ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Reverse Phase ◽  
Phase Partition ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract Methapyrilene hydrochloride (MP·HCl) was extracted from feed with methanol and determined by reverse phase partition chromatography in less than 15 min, using isocratic elution with acetonitrile-1.1% ammonium carbonate (1 + 1) as the mobile phase. This procedure was tested on feed treated with MP·HCl at levels of 125,500, and 2000 ppm. Recoveries were 104,95, and 96% with coefficients of variation of 2.4,1.6, and 0.6%, respectively. MP·HCl in feed was stable for 14 days. This method was also successfully used to determine MP·HCl in 3 sleep aid tablets.

Liquid Chromatographic Determination of Bendiocarb in Technical Materials and Wettable Powder Formulations: Collaborative Study

1986 ◽  
Vol 69 (5) ◽  
pp. 908-911
Author(s):  
Peter L Carter ◽  
Keith C Overton ◽  
◽  
P G Baker ◽  
O O Bennett ◽  
...  
Keyword(s):  
Statistical Data ◽  
Collaborative Study ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Liquid Chromatograph ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A liquid chromatographic method for determination of bendiocarb in technical materials and wettable powders was tested by 12 collaborators. Bendiocarb is dissolved in acetonitrile containing 0.1% propiophenone as internal standard. This solution is analyzed on a liquid chromatograph utilizing a reverse phase (C18) column. The compound is detected at 254 nm and peak area is used for quantitation. The 3 different materials studied contained 20, 80, and nominally 100% bendiocarb. Each was examined in duplicate to provide the necessary matched pairs. Collaborators approved of the ease and simplicity of the method and, in particular, the way the method can be applied to automatic injection assemblies. The statistical data show acceptable precision of the method: Reproducibility coefficients of variation were 20% material, 2.04%; 80% material, 1.02%; and nominal 100% material (technical product), 0.64%. The method has been adopted official first action.

High Performance Liquid Chromatographic Determination of Difenzoquat Residues in Water

1982 ◽  
Vol 65 (5) ◽  
pp. 1097-1101
Author(s):  
Ijaz Ahmad
Keyword(s):  
Water Samples ◽  
High Performance ◽  
Tap Water ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Methyl Sulfate ◽  
Liquid Chromatograph ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A simple analytical method is described for the quantitative determination of difenzoquat (1,2- dimethyl-3,5-diphenyl-lH-pyrazolium methyl sulfate) residues in water. The method involves high performance liquid chromatography with ultraviolet detection at 255 nm. The procedure is used to determine 2 ppb to 1 ppm levels of difenzoquat in pure and tap water. Samples which contain ≥50 ppb difenzoquat are injected directly into the liquid chromatograph without prior separation, concentration, or purification. Samples containing ≤50 ppb difenzoquat are first enriched on C18 Sep-Pak reverse phase cartridges and then injected into the liquid chromatograph. Average recoveries of difenzoquat were greater than 92% with a coefficient of variation less than 4.5%. The method can be used for water samples with difenzoquat concentrations as low as 2 ppb.

High Performance Liquid Chromatographic Determination of α-Tocopherol in Fish Liver

1980 ◽  
Vol 63 (4) ◽  
pp. 889-893 ◽  
Author(s):  
Silas S O Hung ◽  
Young C Cho ◽  
Stanley J Slinger
Keyword(s):  
High Performance ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Peak Height ◽  
Fish Liver ◽  
Liver Sample ◽  
Liquid Chromatograph ◽  
Simple Method ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic

Abstract A simple method is described for the determinatio n of α-tocopherol in fish liver by high performance liquid chromatography. This method does not involve saponification or thin layer chromatography and thus avoids the destruction of α-tocopherol during sample preparation. The homogenized liver sample is extracted twice with dioxane–isooctane (20+80, v/v), and the combined extracts are dried under vacuum. The residue is extracted 3 times with acetonitrile from which α-tocopherol is then extracted with isooctane. The residue from the dried isooctane solution is dissolved in methanol–water (90+10, v/v) which is injected directly onto a micro Bondapak C18 high performance liquid chromatograph. The detection response to α-tocopherol at 280 nm was measured by peak height which was linear from 1 to 10 μg/25 μL injection. The coefficients of variation for retention time and peak height for 5 replicate analyses of the standard during 2 weeks were 1.4 and 2.4%, respectively. Recovery of α-tocopherol added to the sample before homogenization was 80–92% with a mean of 86.2% and a coefficient of variation of 4.9%. The minimum amount of sample and the concentration of α-tocopherol that can be accurately determined by the method are 0.5 g liver and 1 μg α-tocopherol/g liver, respectively.

High-Performance Liquid Chromatographic Determination of Strychnine in Grain Baits

1975 ◽  
Vol 58 (5) ◽  
pp. 957-960 ◽  
Author(s):  
Rodney J Bushway ◽  
Christine W Cramer ◽  
Alan R Hanks ◽  
Billy M Colvin
Keyword(s):  
High Performance ◽  
High Resolution Mass Spectrometry ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Commercial Sample ◽  
Liquid Chromatograph ◽  
Chromatographic Procedure ◽  
Stainless Steel Column ◽  
Liquid Chromatographic

Abstract A simple and rapid high-performance liquid chromatographic procedure is described for the determination of strychnine. Grain baits containing strychnine alkaloid are ground, mixed, and extracted by shaking with chloroform. Without further cleanup, extract nitrates are injected directly into a liquid chromatograph. Chromatography is complete within 7 min and peak heights are used for quantitation. Separations were made on a 30 cm × 4 mm id stainless steel column packed with μ Porasil (8–12 μm silica). The eluting solvent was methanolchloroform (10+90) at a flow rate of 2.0 ml/ min. Recovery of spiked samples ranged from 91.5 to 95.2%. Confirmation of strychnine from a commercial sample was made by high resolution mass spectrometry with mass agreement to 1.2 ppm.

High Performance Liquid Chromatographic Method for Determination of Temephos in Technical and Formulated Products: Collaborative Study

1982 ◽  
Vol 65 (3) ◽  
pp. 580-583
Author(s):  
James W Miles ◽  
Dwight L Mount
Keyword(s):  
Ethyl Acetate ◽  
High Performance ◽  
Collaborative Study ◽  
Internal Standard ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Water Dispersible ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic

Abstract An HPLC method for the determination of temephos in temephos technical and formulated products has been subjected to an international collaborative study with 14 laboratories participating. Samples were extracted with ethyl acetate and eluted on a silica gel column with ethyl acetate-hexane (1 + 9); p-nitrophenyl p-nitrobenzoate served as the internal standard. Collaborators were furnished samples of technical, 20 and 50% emulsifiable concentrates, 50% water-dispersible powder, and 1% sand granules. The coefficients of variation of the values obtained on the 5 samples were 1.21,2.02,1.26,1.89, and 9.90%, respectively. The method has been adopted official first action.

High Performance Liquid Chromatographic Determination of Lactose in Milk

1981 ◽  
Vol 64 (4) ◽  
pp. 805-807
Author(s):  
Leslie G West ◽  
Marie A Llorente
Keyword(s):  
High Performance ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Chocolate Milk ◽  
Silica Column ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A rapid and simple high performance liquid chromatographic method for the determination of lactose in milk was developed. Samples were diluted with 0.5% perchloric acid and centrifuged, and an aliquot of the supernate was mixed with acetonitrile. Lactose was separated on a 10 μm particle-size silica column with aqueous acetonitrile as the mobile phase. The recovery of lactose from whole, skim, and chocolate milk averaged 99.2, 101.1, and 100.4%, respectively. Coefficients of variation for routinely performed duplicate determinations are between 1.0 and 1.5%.

High Performance Liquid Chromatographic Determination of Caffeine in Decaffeinated Coffee, Tea, and Beverage Products

1983 ◽  
Vol 66 (3) ◽  
pp. 606-609 ◽  
Author(s):  
Samy H Ashoor ◽  
George J Seperich ◽  
Woodrow C Monte ◽  
Jim Welty
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Uv Detector ◽  
Coefficients Of Variation ◽  
Decaffeinated Coffee ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A method was developed for determining caffeine in decaffeinated coffee, tea, and beverage products by high performance liquid chromatography (HPLC). The HPLC system consisted of a Bio-Sil ODS-5S C18 column, methanol-water (25 + 75) mobile phase at 1 mL/min, and a UV detector. The method is simple and specific. Caffeine recoveries were 93.8-98.3% and coefficients of variation were 0.90-2.25%.

High Performance Liquid Chromatographic Determination of Sulfanilic Add, Schaeffer’s Salt, 4,4´-(Diazoamino)-DibenzenensuIfonic Acid, and 6,6´-Oxybis(2-Naphthalenesulfonic Acid) in FD&C Yellow No. 6: Collaborative Study

1980 ◽  
Vol 63 (1) ◽  
pp. 61-68
Author(s):  
Elizabeth A Cox ◽  
◽  
R Beswick ◽  
L Bille ◽  
G Gasper ◽  
...  
Keyword(s):  
High Performance ◽  
Collaborative Study ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Sulfanilic Acid ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic Determination ◽  
Standard Deviations ◽  
Liquid Chromatographic

Abstract Eight laboratories participated in a collaborative study of a high performance liquid chromatographic procedure for determining sulfanilic acid, Schaeffer's salt, 4,4´-(diazoamino)-dibenzenesulfonic acid (DAADBSA), and 6,6´-oxybis(2-naphthalenesulfonic acid) (DONS) in FD&C Yellow No. 6. The standard deviations for one analysis in any one laboratory for sulfanilic acid at 0.2%, Schaeffer's salt at 0.26%, DAADBSA at 0.1%, and DONS at 1.0% were 0.015%, 0.014%, 0.018%, and 0.077%, respectively. The method has been adopted as official first action.

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