Illicit heroin manufacturing by-products: capillary gas chromatographic determination and structural elucidation of narcotine- and norlaudanosine-related compounds

1984 ◽  
Vol 56 (14) ◽  
pp. 2940-2947 ◽  
Author(s):  
Andrew C. Allen ◽  
Donald A. Cooper ◽  
James M. Moore ◽  
Manfred. Gloger ◽  
Helmut. Neumann
Keyword(s):  
Chromatographic Determination ◽  
Structural Elucidation ◽  
Related Compounds ◽  
By Products

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.

Synthesis of 5-n-alkylresorcinol dimethyl ethers and related compounds via substituted thiophens

1971 ◽  
Vol 24 (12) ◽  
pp. 2655 ◽  
Author(s):  
D Buddhasukh ◽  
JR Cannon ◽  
BW Metcalf ◽  
AJ Power
Keyword(s):  
Raney Nickel ◽  
Stannic Chloride ◽  
Electrophilic Attack ◽  
Related Compounds ◽  
By Products

5-n-Alkylresorcinol dimethyl ethers have been synthesized by desulphurization of 2-(3,5-dimethoxybenzyl)-5-n-alkylthiophens with Raney nickel. The method has been adapted to the preparation of 9-(3,6- dimethoxyphenyl)nonyl alcohol which has been converted into both (2)- and (E)-15-(3,5-dimethoxyphenyl)pentadec-5-ene. ��� Friedel-Crafts acylation of 2-(3,5-dimethoxybenzyl)thiophen with n- hexoyl chloride, or with n-decoyl chloride, in the presence of stannic chloride, yielded the expected 2-(3,6-dimethoxybenzyl)-5-n- acylthiophens, but by-products were formed as the result of competing electrophilic attack on the 3,5-dimethoxybenzyl moiety. The chief by- products, which arise by subsequent Bradsher cyclodehydration, have been formulated as 5,7-dimethoxy-4-n-alkylnaphtho[2,3-b]thiophens. ��� An attempt to synthesize 1,14-bis(3,5-dimethoxyphenyl)tetradecane from 2,2?,6?,2?-terthienyl by an adaptation of this method was unsuccessful.

Chromatographic determination of benz[c]acridines and related compounds in airborne carcinogens

1995 ◽  
Vol 710 (1) ◽  
pp. 117-128 ◽  
Author(s):  
Noboru Motohashi ◽  
Roger Meyer ◽  
Joseph Molnár ◽  
Cyril Párkányi ◽  
Xingchun Fang
Keyword(s):  
Chromatographic Determination ◽  
Related Compounds

Gas Chromatographic Determination of Fenvalerate Insecticide Residues in Processed Tomato Products and By-Products

1984 ◽  
Vol 67 (4) ◽  
pp. 824-826
Author(s):  
Terry D Spittler ◽  
Robert J Argauer ◽  
Donald J Lisk ◽  
Ralph O Mumma ◽  
George Winnett ◽  
...  
Keyword(s):  
Chromatographic Analysis ◽  
Fresh Produce ◽  
Chromatographic Determination ◽  
Synthetic Pyrethroid ◽  
Analytical Technique ◽  
Insecticide Residues ◽  
Collaborative Agreement ◽  
Tomato Products ◽  
By Products

Abstract The results of a 5-laboratory collaborative determination of residues of the synthetic pyrethroid insecticide fenvalerate in tomato products are presented. Tomatoes from plants treated in the field at 2-4 day intervals (13 foliar applications) were processed into chopped fresh tomatoes, canned quarters, juice, paste, and the by-product skins plus seeds. Gas chromatographic analysis of the commodities for fenvalerate showed the fresh produce to contain 0.26 ppm, and the skins plus seeds contained 1.9 ppm. Residues were barely detectable in canned peeled quarters and juice, but averaged 0.12 ppm for paste, the concentration product of juice. High residues were associated with the skin content of the product. Five laboratories using modifications of the same analytical technique obtained good collaborative agreement.

Gas-Liquid Chromatographic Determination of Fenvalerate Insecticide Residues in Processed Apple Products and By-Products

1982 ◽  
Vol 65 (5) ◽  
pp. 1106-1111
Author(s):  
Terry D Spittler ◽  
Robert J Argauer ◽  
Donald J Lisk ◽  
Ralph O Mumma ◽  
George Winnett ◽  
...  
Keyword(s):  
Chromatographic Analysis ◽  
Chromatographic Determination ◽  
Synthetic Pyrethroid ◽  
Insecticide Residues ◽  
Apple Products ◽  
Liquid Chromatographic Analysis ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
By Products

Abstract Apples from trees treated in the field at 2-week intervals (9 foliar applications) with the synthetic pyrethroid insecticide fenvalerate (cyano(3-phenoxyphenyL)methyl 4-chloro-alpha-(1-methylethyl)- benzeneacetate) were processed into apple sauce, juice, pomace, and peels plus cores. Gas-liquid chromatographic analysis of the commodities for fenvalerate showed the sauce and juice to be essentially residue-free, the whole apples to contain about 0.4 ppm, and the pomace and peels plus cores to contain about 2 and 1.5 ppm, respectively. Agreement among 5 laboratories using modifications of the same basic method was good.

Liquid Chromatographic Determination of Residual Reactants and Reaction By-Products in Polyethylene Terephthalate

1989 ◽  
Vol 72 (3) ◽  
pp. 468-470 ◽  
Author(s):  
Timothy H Begley ◽  
Henry C Hollifield
Keyword(s):  
Polyethylene Terephthalate ◽  
Terephthalic Acid ◽  
Chromatographic Determination ◽  
Cyclic Trimer ◽  
Food Packages ◽  
Precipitation Procedure ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
By Products

Abstract A precipitation procedure and liquid chromatography (LC) were used to measure the residual reactants and reaction by-products in polyethylene terephthalate (PET) polymers and food packages. The polymer is dissolved in l,l,l,3,3,3-hexafluoro-2-propanol/methyIene chloride and then precipitated with acetone. The filtered solution is evaporated almost to dryness, and the concentrate is diluted with dimethylacetamide for LC analysis. Recoveries for terephthalic acid (TA), bis(2-hydroxyethyl) terephthalate (BHET), and the PET cyclic trimer averaged 95,104, and 98%, respectively. The residual levels of TA, BHET, monohydroxy ethylene terephthalic acid, and the PET cyclic trimer were measured in commercial resins and food packages.

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