Liquid Chromatographic Separation and Fluorometric Determination of cw- and frans-Isoeugenol in Perfumes, Colognes, and Toilet Waters

1988 ◽  
Vol 71 (4) ◽  
pp. 818-820
Author(s):  
Harris H Wisneski ◽  
Ronald L Yates ◽  
John A Wenninger

Abstract A liquid chromatographic (LC)-fluorometric method is described for the determination of cis- and frans-isoeugenol (2-methoxy-4-propenylphenol) in perfumes, colognes, and toilet waters. A test portion of the product is added to diethyl ether, and the isoeugenol isomers are extracted with sodium hydroxide solution. The basic extract is then acidified, and the isoeugenol isomers are extracted with isooctane. Aliquots of the isooctane extract are analyzed by using a silver ion cation exchange LC column interfaced to a spectrophotofluorometer. Each isomer in the product is determined by comparing its fluorescence emission intensity with that of an external standard consisting of a mixture of both isomers in which the relative concentration of each has been determined. Average recoveries from various commercial fragrances fortified with a mixture of cis- and trans-isoeugenol with total isoeugenol content of 0.1,0.5, and 4.0 mg/mL ranged from 87 to 105% for the taww-isomer (SD = 4.6%) and from 83 to 113% for the cw-isomer (SD = 6.7%). The limit of determination is approximately 0.002 mg/mL.

1988 ◽  
Vol 71 (4) ◽  
pp. 821-823
Author(s):  
Harris H Wisneski ◽  
Ronald L Yates ◽  
John A Wenninger

Abstract A liquid chromatographic (LC) method is described for the determination of cinnamyl alcohol (3-phenyl-2-propen-l-ol) in fragrance compositions. The fragrance product is partially cleaned up by diluting the fragrance with a 95% ethanol-water mixture and passing it through a short column containing RP-8 packing. An aliquot of the effluent is then analyzed by LC using an RP-18 column interfaced to a spectrophotofluorometer equipped with double monochromators. The fluorescence emission intensity of the eluted cinnamyl alcohol is measured and compared with that of a standard to calculate the amount of cinnamyl alcohol present. Recoveries from fragrance products fortified with cinnamyl alcohol at levels ranging from 0.0020 to 0.060 mg/mL ranged from 85 to 105% with a mean of 94%. The lowest level of determination was 0.0005 mg/mL.


1996 ◽  
Vol 79 (4) ◽  
pp. 883-888 ◽  
Author(s):  
Mary W Trucksess ◽  
Duwayne E Ready ◽  
Marie K Pender ◽  
Cathy A Ligmond ◽  
Garnett E Wood ◽  
...  

Abstract A liquid chromatographic (LC) method for determining deoxynivalenol (DON) in white flour, whole wheat flour, and bran was developed. A 25 g test portion was extracted with acetonitrile-water (84 + 16), and the extract was filtered and applied to a column containing a combination of charcoal, Celite, and other adsorbents. The eluate was then chromatographed on a silica-based, reversedphase LC column by using a gradient of water and methanol. DON was measured at 220 nm. Average recoveries of DON from white flour, whole wheat flour, and bran spiked at 1 fig/g were 88,86, and 85%, respectively. The limit of determination of the method was <0.5 μg/g. A total of 562 wheat-based products from the 1993 crop year were collected by 21 U.S. Food and Drug Administration District Offices and analyzed by this method in Kansas City, Seattle, and New Orleans District Laboratories. The numbers of samples with DON contamination ≥1 μg/g from 163 bran, 272 white flour, 90 whole wheat flour, and 37 miscellaneous test samples were 20,28,14, and 2, respectively. About 52,50,40, and 27% of the same test samples were contaminated with DON at levels ≥0.1 μg/g.


2012 ◽  
Vol 70 (4) ◽  
pp. 296-302 ◽  
Author(s):  
Victor Abrahamsson ◽  
Signe Hoff ◽  
Nikoline J. Nielsen ◽  
Marianne N. Lund ◽  
Mogens L. Andersen

2001 ◽  
Vol 84 (1) ◽  
pp. 43-46 ◽  
Author(s):  
Yuzo Yamamoto ◽  
Fusao Kondo

Abstract A liquid chromatographic (LC) method was developed for simultaneous measurement of halofuginone (HFN) and amprolium (APL) in chicken muscle and egg. HFN and APL were extracted from chicken muscle and egg with acetonitrile. In chicken egg, they were partially purified by solid-phase extraction (SPE) to separate them from impurities. The LC separation was performed on a 4.6 mm id × 250 mm TSK-gel ODS-80TM column using acetonitrile–McIlvaine buffer, pH 3.4, containing 0.01M sodium lauryl sulfate (42 + 58) as the mobile phase. Ultraviolet detection of HFN and APL was performed at wavelengths of 242 and 265 nm, respectively. Recoveries of HFN and APL from chicken muscle spiked at 0.5 μg/g were 74.8 ± 17.7 and 94.2 ± 5.0%, respectively (mean ± standard deviation [SD], n = 10). In chicken muscle, the lower limit of determination for both APL and HFN was 0.03 μg/g. Recoveries of HFN and APL from chicken egg spiked at 0.5 μg/g by a cleanup procedure using SPE were 54.6 ± 3.4 and 85.0 ± 2.4%, respectively (mean ± SD, n = 5). In chicken egg, the lower limit of determination for both APL and HFN was 0.04 μg/g.


1999 ◽  
Vol 82 (5) ◽  
pp. 1214-1216 ◽  
Author(s):  
G Anthony Ohmes ◽  
Thomas C Mueller

Abstract A rapid method for the determination of sulfentrazone in soils is described. The method consists of extraction of soil samples with methanol, filtration, liquid chromatographic separation of methanol-soluble components through a C18 column, and ultraviolet detection at 220 nm. Recoveries from fortified surface soils were >85% for sulfentrazone. Average relative standard deviations over the soils examined was 7.7%. A conservative lower limit of quantitation for sulfentrazone was 40 ng/g soil.


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