High Performance Liquid Chromatographic Analysis of Rotenone Formulations: Collaborative Study

1983 ◽  
Vol 66 (3) ◽  
pp. 796-800
Author(s):  
Rodney J Bushway ◽  
◽  
M J Bennett ◽  
W R Betker ◽  
R Bolduc ◽  
...  
Keyword(s):  
High Performance ◽  
Collaborative Study ◽  
High Performance Liquid Chromatographic ◽  
Peak Height ◽  
Hplc Method ◽  
Reverse Phase Hplc ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic Analysis ◽  
Infrared Method ◽  
Liquid Chromatographic

Abstract A collaborative study was conducted on a high performance liquid chromatographic (HPLC) method for determining rotenone in formulations. One liquid and 4 dust samples, containing other rotenoids and pesticides, with rotenone guarantees ranging from 0.75% to 20% were analyzed by 16 laboratories. Peak height measurements were used by 14 laboratories while 8 laboratories used integrator area measurements. Samples were extracted on a rotary shaker for 1% h with dioxane. An aliquot was analyzed using reverse phase HPLC and UV detection at 280 nm. Coefficients of variation ranged from 2.47 to 3.19% for peak height determinations and from 2.56 to 6.00% for peak area determinations. One collaborator analyzed the samples by the official infrared method for a comparison. The HPLC method has been adopted official first action.

High Performance Liquid Chromatography of Aflatoxins in Cottonseed Products

1977 ◽  
Vol 60 (1) ◽  
pp. 89-95 ◽  
Author(s):  
Walter A Pons ◽  
Anthony O Franz
Keyword(s):  
Silica Gel ◽  
High Performance ◽  
Methylene Chloride ◽  
High Performance Liquid Chromatographic ◽  
Peak Height ◽  
Hplc Method ◽  
Coefficients Of Variation ◽  
Water Saturated ◽  
High Degree ◽  
Liquid Chromatographic

Abstract A precise and sensitive high performance liquid chromatographic (HPLC) method is proposed for determining aflatoxins in cottonseed products in 1.0—1.5 hr. After aqueous acetone extraction, lead acetate treatment, and partition of aflatoxins into methylene chloride, sample extracts are purified on a small silica gel column requiring only 125 ml solvent/sample. Aflatoxins B1 and B2 in the purified extract are resolved on a micro particulate (10 μm) silica gel column in ca 8 min, using a water-saturated chloroform - cyclohexane - acetonitrile solvent, with detection by ultraviolet absorbance at 365 nm. The resolution was highly reproducible, giving coefficients of variation of 0.2—1.0% for retention and 1.0—2.3% for quantitation. Recovery of added aflatoxins B1 and B2 was 90— 95% at levels of 5—100 μg/kg. The within-laboratory coefficients of variation of the entire method, based on repetitive assays of a cottonseed meal (34 μg B1/kg, 6 μg B2/kg), were 7.3% (B1) and 7.4% (B3). A high degree of correlation was obtained for HPLC estimation by 2 different commercial columns; for quantitation by peak height vs. electronic integration; and for quantitation by HPLC or thin layer chromatography.

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 Analysis of Supplemental Vitamin E in Feed

1977 ◽  
Vol 60 (1) ◽  
pp. 137-139
Author(s):  
Badaruddin Shaikh ◽  
Hsinkuang S Huang ◽  
Walter L Zielinski
Keyword(s):  
Vitamin E ◽  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Peak Height ◽  
Phase Detection ◽  
Coefficients Of Variation ◽  
Supplemental Vitamin ◽  
One Step ◽  
Liquid Chromatographic Analysis ◽  
Liquid Chromatographic

Abstract Supplemental vitamin E is extracted from feed in one step with methanol and analyzed by reverse phase partition chromatography in less than 10 min, using isocratic elution with either methanol or water-methanol as the mobile phase. Detection response (as measured by peak area) was linear between 0.5 and 3.0 μg, and the coefficients of variation for retention time and peak height on replicate analyses of the standard sample were 0.8 and 2.3%, respectively.

Analysis of Fat-Soluble Vitamins. XXII. High Performance Liquid Chromatographic Determination of Vitamin D in Concentrates. Collaborative Study1

1979 ◽  
Vol 62 (5) ◽  
pp. 1031-1040
Author(s):  
Frits J Mulder ◽  
Ellen J De Vries ◽  
Ben Borsje
Keyword(s):  
Vitamin D ◽  
High Performance ◽  
Chemical Method ◽  
Collaborative Study ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
De Vries ◽  
Fat Soluble Vitamins ◽  
Liquid Chromatographic

Abstract A collaborative study was carried out which compared the official chemical method (43.B14- 43.B24), the HPLC method according to Hofsass et al. including maleic anhydride treatment, and the HLPC procedure according to De Vries et al. for vitamin D concentrates. A total of 396 samples were distributed to 33 collaborators for analysis. Five laboratories performed both the chemical and the HPLC methods. Five laboratories performed the Hofsass method and 16 laboratories performed the De Vries method. The results for the chemical method agreed with the theoretical values for the samples, and the standard deviation was comparable to that obtained in previous AOAC collaborative studies. Collaborative results for the Hofsass method were low. In addition, incorrect use of a fixed conversion factor (1/0.586) and necessity of a double chromatographic system on a non-treated and a treated vitamin D sample reduce the effectiveness of the method. There were no adverse reactions to the De Vries HPLC method. It is recommended that the method be adopted official first action as an alternative procedure for determining vitamin D in concentrates, excluding powders containing irradiated 7-dehydrocholesterol.

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.

Liquid chromatographic analysis of disopyramide and its mono-N-dealkylated metabolite.

1979 ◽  
Vol 25 (3) ◽  
pp. 405-408 ◽  
Author(s):  
J J Lima
Keyword(s):  
Chromatographic Analysis ◽  
Mobile Phase ◽  
High Performance ◽  
Antiarrhythmic Drugs ◽  
Internal Standard ◽  
High Performance Liquid Chromatographic ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic Analysis ◽  
Liquid Chromatographic ◽  
Lower Limits

Abstract We describe a rapid, sensitive, and specific "high performance" liquid chromatographic analysis for disopyramide and its mono-N-dealkylated metabolite in serum, urine, and saliva. We used a mu-Bondapak CN column and an acetate buffer mobile phase containing methanol. Retention times for the two compounds and the internal standard, p-chlorodisopyramide, were 3.4, 4.1, and 6.3 min, respectively. The lower limits of sensitivity for drug and metabolite were 50 and 80 micrograms/L, respectively, with maximum coefficients of variation of 4.6 and 12%, respectively. Currently used antiarrhythmic drugs did not interfere with the analysis of disopyramide, and the pharmacokinetics of the drug, obtained from studies of one subject, agree well with reported values.

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 Analysis of Diflubenzuron and Its Formulations: Collaborative Study

1983 ◽  
Vol 66 (2) ◽  
pp. 312-316 ◽  
Author(s):  
Bram Van Rossum ◽  
Albertus Martijn ◽  
Albert A De Reijke ◽  
Jakob Zeeman ◽  
◽  
...  
Keyword(s):  
Chromatographic Analysis ◽  
High Performance ◽  
Collaborative Study ◽  
Internal Standard ◽  
High Performance Liquid Chromatographic ◽  
Water Dispersible ◽  
Liquid Chromatographic Method ◽  
Powder Samples ◽  
Liquid Chromatographic Analysis ◽  
Liquid Chromatographic

Abstract Diflubenzuron 90% pre-concentrate and its 25% water-dispersible powder were analyzed by a high performance liquid chromatographic method. Six samples were extracted with 1,4-dioxane, linuron was added as internal standard, and diflubenzuron was separated on a 25 cm × 4.6 mm column packed with Zorbax BP-C8 with acetonitrile-water-l,4-dioxane (450 + 450 + 100) at 1.3 mL/min and monitored at 254 nm. Results were obtained from 17 laboratories. Within-laboratory repeatability was 0.6% for both the pre-concentrate and the water-dispersible powder samples and the reproducibility was 1.2%. The method has been adopted as a full CIPAC method and was adopted official first action by AOAC.

scholarly journals Simple Quantification of Pentosidine in Human Urine and Plasma by High-Performance Liquid Chromatography

2017 ◽  
Vol 2017 ◽  
pp. 1-6 ◽  
Author(s):  
Ji Sang Lee ◽  
Yoon-Sok Chung ◽  
Sun Young Chang ◽  
Yi-Sook Jung ◽  
So Hee Kim
Keyword(s):  
Human Urine ◽  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Diabetic Patients ◽  
Gradient System ◽  
Coefficients Of Variation ◽  
Relative Errors ◽  
Liquid Chromatographic ◽  
Lower Limits

Pentosidine is an advanced glycation end-product (AGE) and fluorescent cross-link compound. A simple high-performance liquid chromatographic (HPLC) method was developed for the detection and quantification of pentosidine in human urine and plasma. The mobile phase used a gradient system to improve separation of pentosidine from endogenous peaks, and chromatograms were monitored by fluorescent detector set at excitation and emission wavelengths of 328 and 378 nm, respectively. The retention time for pentosidine was 24.3 min and the lower limits of quantification (LLOQ) in human urine and plasma were 1 nM. The intraday assay precisions (coefficients of variation) were generally low and found to be in the range of 5.19–7.49% and 4.96–8.78% for human urine and plasma, respectively. The corresponding values of the interday assay precisions were 9.45% and 4.27%. Accuracies (relative errors) ranged from 87.9% to 115%. Pentosidine was stable in a range of pH solutions, human urine, and plasma. In summary, this HPLC method can be applied in future preclinical and clinical evaluation of pentosidine in the diabetic patients.

scholarly journals High Performance Liquid Chromatographic Analysis of Rutin in Allium Species from Bosnia and Herzegovina

2020 ◽  
Vol 69 (11-12) ◽  
pp. 647-651
Author(s):  
Mirsada Salihović ◽  
Emin Sofić
Keyword(s):  
Bosnia And Herzegovina ◽  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Allium Species ◽  
Beneficial Effects ◽  
Liquid Chromatographic Analysis ◽  
Liquid Chromatographic ◽  
Harmful Effects ◽  
Capillary Walls

Rutin is quercetin heteroside widely present in plants that exhibit many health-beneficial effects, such as strengthening the capillary walls, reducing the harmful effects of LDL cholesterol, and reducing the risk of cardiovascular diseases. Rutin was determined from three <i>Allium</i> species (<i>A. cepa</i>, <i>A. sativum</i>, and <i>A. ursinum</i>) collected in Bosnia and Herzegovina by the HPLC method associated with electrochemical detection. The analysis was performed from methanol extracts of bulb and leaf of garlic, bulb and leaf of onion, and leaves of wood garlic. Rutin was present in all of the examined samples. The highest rutin content was found in garlic leaves (0.78 ± 0.09 mg g<sup>–1</sup>), and the lowest in onion bulbs (0.04 ± 0.10 mg g<sup>–1</sup>). The contents of rutin were higher in leaf samples, suggesting that leaves of onion and garlic are recommended as a better natural source of this glycoside.

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