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PME RESEARCH LABORATORY, November 1979 1 r l PROJECT TITLE ANALYTICAL INVESTIGATIONS PERIiOD COVERED . NOVEMBER 1979 WRITTEN!BY . K.D. BRUNNEMANN' I. SORBATE ASSAY During the finalphase of this project, the question arose whether sorbate is transferredifrom the filler into the smoke. When spraying sorbate onto tobacco, we observed a transfer rate of 11.2% in plain cigarettes (1). In another experiment, sorbate was injected into cigarettes (PMM) and a transfer rate of 12.9 to 14.11% was observed. (This transfer rate is similar to that of nicotine.) When the filter was removed, the transfer rate rose to 21.4%; the filter from the PMM cigarettes contained 4.3% of the sorbate. The sorbate study was presentedat the 33rd TCRC (2). II. COUMARIN ASSAY Since we observed that coumarin canibe analyzed simultaneously with sorbate using the sorbate procedure (3), we were also interested to determine the precision of the coumarin assay. When analyzing a coumarin-contai~ning pipe tobacco five times, the precision was found to be 1.6% which is comparable with that of sorbate (1.5%; 4). In conclusion, the assay procedure developed can be applied to sorbate or coumarin or both. NNN ASSAY The tubular oven constructed recently (5) showed some initial temperature oscililations resulting in inconsistent detector responses (up to 8% variation). This was overcome by using a reduce&voltage which decreased the frequency of the osciL- lations. Also, the overalli pyrolysis temperature has been reduced to achieve better consistency. The variation is now 2% under these conditions. A calibration curve of NNN andi NNK has been made and found acceptable. A gas chromatogram separating NNN and NNK is shown in Fig, 1. The prominent peak before NNN is dihexylnitrosamine (internal standard),. It is planned to have an extensive sample survey when the method will have been finalized. Using NNN-14C, we find a recovery of 901- 100%. - 5 - I

PME RESEARCH LABORATORY, November 1979 IV. MISCELLANEOUS October 29-31 : 33rd Tobacco Chemists' Research Conference (TCRC), Lexington, Kentucky. Abstracts of 60 papers are available. November 1-2 : Visit to Philip Morris USA, Richmond, Virginiz November 6 : Visit to the New England I~nstitute for Life Sciences, Waltham, Massachusetts. Discussions on Thermosorb cartridge and table-top TEA. A detailed report is availablie on request. November 7 : Visit to the Naylor Dana Institute, Valhalla, • New York. Discussion on their ongoing research program. A detailed report is also available on request. REFERENCES (1) PME Research Laboratory, Monthly Progress Report, October 1979 P. 10 (2) K.D. Brunnemann, Routine HPLC Method for Assessing Sorbate in Tobacco. Presented at the 33rd TCRC, Lexington, Kentuc' October 29-31, 11979, Abstract No. 61 (3) PME Research Laboratory, Monthly Progress Report, June 1979, p. 13 (4) PME Research Laboratory, Monthly Progress Report, July 1979, P - 9 (5) PME Research Laboratory, Monthly Progress Report, October 1979 p. 9 K.D. Brunnemann - 6 -

I 1 FF I GURE 1. GAS CHROMATOGRAM OF NH AND NNK.