scholarly journals Liquid Chromatographic Determination of Safrole in Sassafras-Derived Herbal Products

1997 ◽  
Vol 80 (5) ◽  
pp. 1023-1028 ◽  
Author(s):  
Marvin Carlson ◽  
Richard Thompson
Keyword(s):  
Chromatographic Determination ◽  
Reversed Phase ◽  
Herbal Extract ◽  
Root Bark ◽  
Herbal Products ◽  
Relative Standard ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Related Compounds

Abstract A liquid chromatographic (LC) method was developed for determining safrole in herbal products derived from sassafras (Sassafras albidumf as well as related compounds such as isosafrole and dihydrosafrole. The procedure involves solvent extraction and isolation of analyte by reversed-phase LC with UV detection at 235 nm. Safrole is resolved from related compounds and other sample constituents including thymol, a component of thyme. A linear concentration range of 0.003-0.200 mg/mL was obtained for safrole, isosafrole, and dihydrosafrole. Limits of detection (LOD) and quantitation (LOQ) were 0.0015 and 0.0051 μg/mL for safrole, 0.0018 and 0.0061 μg/mL for isosafrole, and 0.0038 and 0.0125 μg/mL for dihydrosafrole, respectively. Intraday relative standard deviations (RSDs) for safrole (n= 5) from various samples ranged from 1.30 to 5.39% at analyte levels of 0.01-1.5%. Safrole contents of 26 samples including root bark powder, leaves, oils, tea concentrate, herbal extract tinctures, and herbal powder capsules ranged from <LOD for most leaf samples to 92.4% for an oil. Recoveries of safrole from fortified samples ranged from 83.6% for an oil to 117.2% for a tincture preparation. Safrole contents of 0.09-4.66 mg/cup were found for brewed teas prepared from sassafras root bark powders and tinctures.

scholarly journals Liquid Chromatographic Determination of the Glycoalkaloids α-Solanine and α-Chaconine in Potato Tubers: NMKL Interlaboratory Study

1997 ◽  
Vol 80 (3) ◽  
pp. 549-554 ◽  
Author(s):  
Karl-Erik Hellenás ◽  
Carina Branzell ◽  
H Poutanen ◽  
T Suortti ◽  
R Kaario ◽  
...  
Keyword(s):  
Collaborative Study ◽  
Chromatographic Determination ◽  
Reversed Phase ◽  
Potato Tubers ◽  
Photometric Detection ◽  
Liquid Chromatographic Method ◽  
Relative Standard ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract Twelve laboratories participated in a collaborative study to evaluate precision parameters of a liquid chromatographic method for analysis of the glycoalkaloids α-solanine and α-chaconine in potato tubers. Samples consisted of frozen potato tuber homogenates distributed as 3 blind duplicates and 3 split-level pairs. The analytical method included aqueous extraction, workup on disposable solidphase extraction cartridges, and reversed-phase chromatography with photometric detection at 202 nm. Results for α-solanine and α-chaconine were received from 10 and 9 laboratories, respectively. Relative standard deviations for reproducibilo ity for α-solanine and α-chaconine were similar, ranging from 8 to 13% in the applied concentration range of 12 to 260 mg/kg fresh weight.

Liquid Chromatographic Determination of 2-Chloro-4-nitroaniline, 2-Naphthol, and 2,4-Dinitroaniline in D&C Red No. 36

1993 ◽  
Vol 76 (2) ◽  
pp. 287-291 ◽  
Author(s):  
Alan L Scher ◽  
Nicholas C Adamo
Keyword(s):  
Chromatographic Determination ◽  
Reversed Phase ◽  
Calibration Data ◽  
Reversed Phase Liquid Chromatography ◽  
Relative Standard ◽  
Liquid Chromatographic Determination ◽  
Phase Liquid ◽  
Liquid Chromatographic ◽  
Cellulose Column

Abstract A method is described for the determination of the intermediates and a related impurity in D&C Red No. 36 by reversed-phase liquid chromatography. This method may be used to ensure that limits set forth in the Code of Federal Regulations on the amounts of these 3 impurities in the color are not exceeded. The pigment is dissolved in boiling dioxane and then precipitated. The filtrate is chromatographed by isocratic elution, and then the column is washed and reequilibrated. Impurities were identified as 2-chloro-4-nitroaniline (2-CI-4-NA), 2-naphthol, and 2,4-dinitroaniline (2,4-DNA) by comparison of their retention times and spectra with those of standards. Peak area calibrations were linear to at least 0.375% 2-CI-4-NA, 1.25% 2-naphthol, and 0.025% 2,4-DNA, all with zero intercepts. At the specification levels, 99% confidence limits were 0.30 ± 0.006% for 2-CI-4-NA, 1.0 ± 0.03% for 2-naphthol, and 0.020 ± 0.0004% for 2,4-DNA. The limits of determination calculated from calibration data were 0.019% for 2-CI-4-NA, 0.10% for 2-naphthol, and 0.0014% for 2,4-DNA at the 99% confidence level. Recoveries were 100-104% for 2-CI-4-NA added to purified D&C Red No. 36,100% for 2-naphthol, and 100-110% for 2,4-DNA; relative standard deviations were 0.8-3.4%. A survey of certified D&C Red No. 36 samples showed that the batches contained higher levels of intermediates than were determined previously by a cellulose column method in which the pigment was not dissolved.

scholarly journals Liquid Chromatographic Determination of Scopolamine, Hyoscyamine, and Phenobarbital in Tablets

1997 ◽  
Vol 80 (2) ◽  
pp. 331-334 ◽  
Author(s):  
Susan Ting
Keyword(s):  
Mobile Phase ◽  
Chromatographic Determination ◽  
Reversed Phase ◽  
Scopolamine Hydrobromide ◽  
Acid Sodium Salt ◽  
Liquid Chromatographic Method ◽  
Relative Standard ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A liquid chromatographic method using a reversed- phase C18 column and octanesulfonic acid sodium salt-methanol as the mobile phase was developed for the simultaneous determination of phenobarbi- tal, scopolamine, and hyoscyamine in tablets. The mixture of the 3 drugs was resolved in <8 min. Detector responses were linear for 10 μL injections of the following: scopolamine hydrobromide, 8.25-206.3 μg/mL; hyoscyamine sulfate, 15.01-750.76 μg/mL; and phenobarbital, 250-751 μg/mL. Recoveries from tablets were 100.8% for scopolamine hydrobromide, 100.1% for hyoscyamine sulfate, and 100.3% for phenobarbital. Replicate injections of scopolamine hydrobromide, hyoscyamine sulfate, and phenobarbital gave an overall relative standard deviation of <1.0% (n = 10). The method detected as little as 3.3 ng scopolamine hydrobromide.

Liquid Chromatographic Determination of Furazolidone in Shrimp

1994 ◽  
Vol 77 (4) ◽  
pp. 901-904 ◽  
Author(s):  
Guy R Stehly ◽  
Steven M Plakas ◽  
Kathleen R El Said
Keyword(s):  
Chromatographic Determination ◽  
Reversed Phase ◽  
Uv Detection ◽  
Relative Standard ◽  
Liquid Chromatographic Determination ◽  
Standard Deviations ◽  
Liquid Chromatographic

Abstract A liquid chromatographic (LC) method was developed for the quantitation of furazolidone residues in shrimp muscle. The shrimp homogenate (1.0 g) is extracted with acetonitrile, and the extract is taken to dryness. The residue is dissolved in acetonitrile, and the solution is passed through alumina and C18 cleanup columns. The eluate is taken to dryness and reconstituted in a suitable solvent for reversed-phase (C18) LC with UV detection at 365 nm. Recoveries of furazolidone from shrimp homogenates spiked from 5 to 80 ng/g ranged from 74.3 to 79.7%, and relative standard deviations (RSDs) were 5.0–8.9%. RSDs for incurred furazolidone quantitated at 5.9 and 9.2 ng/g were 6.6 and 7.6%, respectively.

Liquid Chromatographic Determination of Glyburide (Glibenclamide) and Its Related Compounds in Raw Materials

1993 ◽  
Vol 76 (5) ◽  
pp. 962-965
Author(s):  
Normand Beaulieu ◽  
Susan J Graham ◽  
Edward G Lovering
Keyword(s):  
Raw Materials ◽  
Chromatographic Determination ◽  
Assay Method ◽  
Liquid Chromatographic Method ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Related Compounds

Abstract A liquid chromatographic method has been developed for the determination of glyburide and 3 known related compounds in drug raw materials. The lower limit of quantitation of the related compounds is about 0.02%. Evaluation of 9 drug raw materials revealed total impurities ranging from 0.17 to 0.65%. The relative standard deviation of the assay method is <1%.

scholarly journals Liquid Chromatographic Determination of Histamine in Fish, Sauerkraut, and Wine: Interlaboratory Study

1998 ◽  
Vol 81 (5) ◽  
pp. 991-998 ◽  
Author(s):  
Paul R Beljaars ◽  
Remmelt Van Dijk ◽  
Klaas M Onker ◽  
Louis J Schout ◽  
◽  
...  
Keyword(s):  
Mobile Phase ◽  
Chromatographic Determination ◽  
Reversed Phase ◽  
Interlaboratory Study ◽  
Relative Standard ◽  
Liquid Chromatographic Determination ◽  
Standard Deviations ◽  
Liquid Chromatographic ◽  
Postcolumn Derivatization

Abstract An interlaboratory study of the liquid chromatographic (LC) determination of histamine in fish, sauerkraut, and wine was conducted. Diminuted and homogenized samples were suspended in water followed by clarification of extracts with perchloric acid, filtration, and dilution with water. After LC separation on a reversed-phase C18 column with phosphate buffer (pH 3.0)-acetonitrile (875 + 125, v/v) as mobile phase, histamine was measured fluorometrically (excitation, 340 nm; emission, 455 nm) in samples and standards after postcolumn derivatization with ophthaldialdehyde (OPA). Fourteen samples (including 6 blind duplicates and 1 split level) containing histamine at about 10- 400 mg/kg or mg/L were analyzed singly according to the proposed procedure by 11 laboratories. Results from one participant were excluded from statistical analysis. For all samples analyzed, repeatability relative standard deviations varied from 2.1 to 5.6%, and reproducibility relative standard deviations ranged from 2.2 to 7.1%. Average recoveries of histamine for this concentration range varied from 94 to 100%

scholarly journals Liquid Chromatographic Determination of S-Adenosyl-L-Methionine in Dietary Supplement Tablets

2002 ◽  
Vol 85 (4) ◽  
pp. 901-905 ◽  
Author(s):  
Joseph Ziqi Zhou ◽  
Ted Waszkuc ◽  
Spiro Garbis ◽  
Felicia Mohammed
Keyword(s):  
Dietary Supplement ◽  
Phosphate Buffer ◽  
Chromatographic Determination ◽  
Reversed Phase ◽  
Ion Pair ◽  
Liquid Chromatographic Method ◽  
Relative Standard ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A simple and reliable liquid chromatographic method was developed for the determination of S-adenosyl-L-methionine (SAM) in dietary supplement tablets. SAM in products was extracted with a phosphate buffer and separated from the mixture on a reversed-phase C8 column by ion-pair chromatography. A gradient mobile phase containing phosphate buffer, sodium octanesulfonate as the ion-pair reagent, and acetonitrile at a flow rate of 1.2 mL/min was used in the analysis. The UV detection wavelength was set at 257 nm. The calibration curve was linear over a range of 75–375 μg/mL for the SAM active ion with R2 = 0.9999. Replicate tests indicated good reproducibility of the method with a relative standard deviation of 0.9% (n = 8). The multiple extractions and recoveries from fortified products showed the high accuracy of the analysis. The use of the acidic buffer for SAM extraction and elution and the use of a fresh standard for each calibration to counteract the instability of the SAM compound significantly improved the accuracy of the method.

Liquid Chromatographic Determination of Bentazon in Technical and Formulated Products: Collaborative Study

1994 ◽  
Vol 77 (2) ◽  
pp. 328-330
Author(s):  
Thomas M Schmitt
Keyword(s):  
Collaborative Study ◽  
Chromatographic Determination ◽  
Reversed Phase ◽  
Relative Standard ◽  
Before And After ◽  
Liquid Chromatographic Determination ◽  
Phase Liquid ◽  
The Mean ◽  
Liquid Chromatographic

Abstract An isocratic reversed-phase liquid chromatographic (LC) procedure for measuring bentazon in commercial herbicide products and aqueous formulations was collaboratively studied by 16 laboratories. Samples are dissolved in LC eluent [0.075M sodium acetate–methanol (60 + 40)] and analyzed by LC on a 30 cm × 3.9 mm octadecylsilyl column with detection by UV absorbance at 340 nm. The quantity of active ingredient is determined by comparing the mean response factor (RF) of the sample to the mean RF of standards injected just before and after each pair of sample injections. The average relative standard deviation (RSDR) for 3 formulations studied was 1.54%; the RSDR for a technical sample was 0.77%. The method has been adopted first action by AOAC INTERNATIONAL.

Continuous Flow and Liquid Chromatographic Determination of p-Toluenesulfonamide in Ice Cream: Interlaboratory Study

1993 ◽  
Vol 76 (3) ◽  
pp. 570-574 ◽  
Author(s):  
Paul R Beljaars ◽  
Remmelt Van Dijk ◽  
Arie Brands ◽  
◽  
M Anderegg ◽  
...  
Keyword(s):  
Continuous Flow ◽  
Collaborative Study ◽  
Ice Cream ◽  
Chromatographic Determination ◽  
Reversed Phase ◽  
Relative Standard ◽  
Liquid Chromatographic Determination ◽  
Standard Deviations ◽  
Liquid Chromatographic

Abstract A collaborative study of the continuous flow (CF) and liquid chromatographic determination of p-toluenesulfonamide (p-TSA) in ice cream was conducted by the Project Group on Collaborative Studies (PCS) of the Inspectorate for Health Protection, Food Inspection Service, The Netherlands. The procedure involves extraction of samples with water followed by cleanup of the extracts by dialysis in the CF system. Dialysates are injected by using a loop injector (500 μL) on a reversed-phase octadecylsilane bonded-phase (C18) column, chromatographed with methanol-water (25 + 75, v/v) as mobile phase, and quantitated by fluorescence detection at 230 nm (excitation) and 295 nm (emission). Seven ice-cream samples containing 0-6.35 mg/kg p-TSA at 4 different levels (1 blank and 3 pairs of split-level samples) were singularly analyzed according to the proposed procedure by 11 laboratories. The data were analyzed by the International Union of Pure and Applied Chemistry/ International Organization for Standardization/ AOAC protocol for statistics. No Cochran and Grubbs outliers were found among the participants. For all samples analyzed, repeatability relative standard deviations (RSDr) varied from 2.08 to 3.67%, whereas the reproducibility relative standard deviations (RSDR) ranged from 7.79 to 11.68%. The average p-TSA values for the split levels 1,2, and 3 were 0.55, 1.02, and 4.44 mg p-TSA/kg, respectively, with mean recoveries ranging from 76 to 79% (overall recovery range for all levels, 63-101%). No false-positive results were reported for the blank sample, and no interference was encountered by the presence of vanilla in samples.

Liquid Chromatographic Determination of Amiodarone Hydrochloride and Related Compounds in Raw Materials and Tablets

1994 ◽  
Vol 77 (6) ◽  
pp. 1447-1453 ◽  
Author(s):  
Pauline M Lacrok ◽  
Norman M Curran ◽  
Wing-Wah Sy ◽  
Dennis K J Goreck ◽  
Pierre Thibault ◽  
...  
Keyword(s):  
Raw Materials ◽  
Chromatographic Determination ◽  
Raw Material ◽  
Liquid Chromatographic Method ◽  
Limit Of Quantitation ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Amiodarone Hydrochloride ◽  
Related Compounds

Abstract A liquid chromatographic method for the determination of amiodarone hydrochloride and 10 related compounds in drug raw material and for assay of drug in tablets was developed. The method specifies a 3 jxm Hypersil nitrile column (150 × 4.6 mm), a mobile phase of 1 + 1 acetonitrile–ammonium acetate buffer (0.1 M adjusted to pH 6.0 with 0.1 M acetic acid), a flow rate of 1 mL/min, and detection at 240 nm. The lower limit of quantitation of the related compounds is 0.02% or less. Drug contents in 2 raw material samples were 100.1 and 99.9% and ranged from 98.2 to 99.4% in 3 tablet formulations. Impurity levels in 2 samples of raw material from different manufacturers were ca 0.4%. The presence of 3 of the known related compounds in these samples was confirmed by liquid chromatographymass spectrometry. The method applied to raw materials was evaluated by a second laboratory and found to be satisfactory.

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