GC_MS
(Hive Addict)
03-12-03 12:34
No 416240
      Impurities in commercially available PMK
(Rated as: excellent)
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Today, I dated some Russian chick, Olga. I just wish I could show you a photograph of her... A single tit fits perfectly in one of my hands, the shape of her erected nipples makes me declaring her as divine, the smell of her pussy makes me hallucinating, and her erotic fantasy is as perverse as mine. Also, she gave me the following article: A Note about some Impurities in Commercially Available Piperonylmethylketone, by AMA Verweij and AGA Sprong.

Introduction - Diketone compounds are known impurities present in the ketones that are used as starting materials in the different syntheses of 3,4-methylenedioxyamphetamine (MDA) and 3,4-methylenedioxymethamphetamine (MDMA) [1]. No further studies have been reported in the literature on impurities present in piperonylmethylketone (PMK) (also known as 3,4-methylenedioxyphenyl-2-propanone), used in the illicit production of MDA. Some of these impurities, and their structures, have been determined in commercially available PMK.

Experimental - Analyses were done on a 1:40 dilution of PMK with chloroform. Gas chromatographic-mass spectral analyses were performed on 1 uL injections using a HP 5971A MSD interfaced with a HP 5890 GC. The MSD was operated in the EI mode. The samples were introduced into the GC via a split injector equipped with a 12.5 m x 0.2 mm id HP Ultra-1 fused silica capillary column with a 0.33 um film thickness. The column temperature was programmed from 100 to 280C at a rate of 10C per minute. The injection port was 275C and the transfer line temperature was 280C. He was used as the carrier gas with a flow rate of about 1 mL/minute.

Results and discussion - The total ion chromatogram (TIC) of a solution of PMK in chloroform is shown in Fig 1 (not included). From the abundance values for the peaks in the TIC shown in Fig 1, the purity of the PMK was estimated to be greater than 95 percent. In the same way, the impurities were found to range from about 0.1 to 1.0 percent. The structure elucidation of the different compounds in the TIC was done by comparing the mass spectral data with different databases [1-3] and applying known fragmentation rules [4,5]. In Table 1, the proposed structures of the impurities together with the mass spectral data are given. All the detected impurities except compounds C and H, have the methylenedioxy group, whereas the other structural differences of the impurities are in the substituents attached to the other side chain of the phenyl group. A trace quantity of safrole, as well as isosafrole, was found, giving rise to the assumption that at least the oxidation of safrole in formic acid by hydrogen peroxide was part of the process of manufacturing PMK. The presence of the oxidation products of PMK, the alcohol and the acid (compounds E and I in table 1), also points to an oxidative process.

References
[1] AMA Verweij. Impurities in illicit drugs preparations: 3,4-(methylenedioxy)amphetamine and 3,4-(methylenedioxy)methamphetamine. Forensic Science Review 4 (1992) 138-146.
[2] Eight Peak Index of Mass Spectra, The Mass Spectra Data Center, The Royal Society of Chemistry. 1983
[3] FW McLafferty, DB Stauffer. The Wiley/NBS Registry of Mass Spectral Data. John Wiley and Sons. 1989
[4] JR Chapman. Practical Organic Mass Spectrometry. John Wiley and Sons. 1985
[5] FW McLafferty, Interpretation of Mass Spectra, University Science Books. 1980

Table 1
[label-name * mol weight * formula]
A-safrole * 162 * C10H10O2
A-isosafrole * 162 * C10H10O2
B-piperonal * 150 * C8H6O3
C-4-allyl-1,2-dimethoxybenzene * 178 * C11H14O2
D-piperonylmethylketone (PMK, main component) * 178 * C10H10O3
E-3,4-methylenedioxyphenyl-2-propanone-(3-ol) * 194 * C10H10O4
F-3,4-methylenedioxyphenyl-1-propanone * 178 * C10H10O3
G-3,4-methylenedioxyphenyl-1-butanone * 172 (sic)* C11H12O3
H-4-isopropyl-1,6-dimethyl-1,2,3,4-tetrahydronaphtalene * 202 * C15H22
I-3,4-methylenedioxyphenylpropionicacid-2-one * 208 * C10H8O5

Abusus non tollit usum
 
 
 
 
    foxy2
(Distinctive Doe)
03-12-03 13:15
No 416252
      Why don't you cite the microgram issue that is  Bookmark   

Why don't you cite the microgram issue that is from.
wink

Or am i mistaken? laugh
 
 
 
 
    GC_MS
(Hive Addict)
03-12-03 13:20
No 416253
      Oops, I forgot ...  Bookmark   

Oops, sorry foxy, forgot to add the source... You know, it's hard to keep yourself concentrated on typing a text while Olga is handling your tools. Want to have a taste?  wink

AMA Verweij, AGA Sprong. A note about some impurities in commercially available piperonylmethylketone. Microgram XXVI(9) (1993) 209

Abusus non tollit usum
 
 
 
 
    Rhodium
(Chief Bee)
03-12-03 14:57
No 416278
      Microgram  Bookmark   

Very nice! Further Microgram articles are very welcome!

This one is now available at ../rhodium/chemistry /mdp2p.impurities.html