Determination of Musk Ambrette in Fragrance Products by Capillary Gas Chromatography with Electron Capture Detection: Interlaboratory Study

1994 ◽  
Vol 77 (6) ◽  
pp. 1467-1471 ◽  
Author(s):  
Harris H Wisneski ◽  
Ronald L Yates ◽  
Donald C Havery
Keyword(s):  
Electron Capture ◽  
Internal Standard ◽  
Fused Silica ◽  
Electron Capture Detection ◽  
Similar Response ◽  
Relative Standard ◽  
Fused Silica Capillary ◽  
Gas Chromatographic Method ◽  
Musk Ambrette

Abstract A gas chromatographic method that uses an internal standard additions technique is described for the determination of musk ambrette (MA) in fragrance products. A solution containing the product and a known amount of an internal standard, musk tibetene (MT), is injected directly into a gas chromatograph equipped with an electron capture detector. The chromatographic separation of the components on a wide-bore fused silica capillary column is recorded and a response constant is calculated from MA and MT peak heights. A similar response constant is also calculated for a standard solution containing known concentrations of MA and MT. The MA content of the fragrance product is then calculated. Average recoveries of MA from fragrance products ranged from 97.6 to 102.3%. The method was also evaluated collaboratively by 6 laboratories. In this study, the reproducibility relative standard deviation for MA in 6 fragrance test samples ranged from 2.78 to 22.87%.

scholarly journals Simultaneous Determination of Residues of Chloramphenicol, Florfenicol, Florfenicol Amine, and Thiamphenicol in Shrimp Tissue by Gas Chromatography with Electron Capture Detection

2000 ◽  
Vol 83 (1) ◽  
pp. 26-30 ◽  
Author(s):  
Allen P Pfenning ◽  
José E Roybal ◽  
Heidi S Rupp ◽  
Sherri B Turnipseed ◽  
Steve A Gonzales ◽  
...  
Keyword(s):  
Ethyl Acetate ◽  
Electron Capture ◽  
Solid Phase ◽  
Internal Standard ◽  
Electron Capture Detection ◽  
Organic Layer ◽  
Standard Curve ◽  
Quantitation Limit ◽  
Relative Standard

Abstract A gas chromatographic (GC) method is presented for determining residues of chloramphenicol (CAP), florfenicol (FF), florfenicol amine (FFa), and thiamphenicol (TAP) in shrimp tissues, with meta-nitrochloramphenicol (mCAP) as the internal standard. The composited shrimp is extracted with basic ethyl acetate, followed by an acetonitrile–basic ethyl acetate mixture. This extract is centrifuged, filtered, evaporated, and reconstituted in water; the reconstituted extract is acidified, defatted with hexane, and passed through a propylsulfonic acid (PRS) and C18 solid-phase extraction (SPE) system. The C18 SPE column is eluted with methanol, and the PRS SPE column is eluted with basic MeOH plus counter ion. The combined eluates are evaporated, reconstituted in acetonitrile, and derivatized with Sylon BFT. After derivatization, the addition of toluene directly to the sample, followed by the addition of basic water, quenches the derivatization process. After centrifugation, the organic layer is carefully removed, and the analytes are determined by GC with electron capture detection. Shrimp tissues were fortified with fenicols (i.e., CAP, FF, FFa, and TAP) at 5, 10, 20, 40, and 80 ng/mL. Overall recoveries were 88, 101, 91, and 84% with overall interassay (between-day) variabilities (i.e., relative standard deviations) of 5.3, 9.4, 12.8, and 7.4% for CAP, FF, FFa, and TAP, respectively. The method detection limits were calculated as 0.7, 1.4, 2.4, and 1.3 ng/g (ppb) for CAP, FF, FFa, and TAP, respectively, based on a 10 g sample. The quantitation limit as determined empirically by this method is the lower limit of the standard curve, which is about 5 ng/g (ppb) for each analyte.

scholarly journals The determination of coumestrol in alfalfa (Medicago sativa) by capillary electrophoresis

2011 ◽  
Vol 48 (No. 5) ◽  
pp. 224-229 ◽  
Author(s):  
J. Moravcová ◽  
T. Kleinová ◽  
R. Loučka
Keyword(s):  
Capillary Electrophoresis ◽  
High Performance ◽  
Solid Phase ◽  
Internal Standard ◽  
Fused Silica ◽  
Detector Response ◽  
Acid Extraction ◽  
Relative Standard ◽  
Fused Silica Capillary

High performance capillary electrophoresis (HPCE) on an uncoated fused-silica capillary column using a&nbsp;borate buffer at pH 9.2 as electrolyte and diode-array detection was developed for the determination of coumestrol in alfalfa. The linear detector response was established in the concentration range 0.76&ndash;140 mg.dm<sup>&ndash;3</sup>, the minimum detectable limit was 0.39 mg.dm<sup>&ndash;3</sup>, and migration time of coumestrol was 5 min. 3-Isobutyl-1-methylxanthin was used as an internal standard. Coumestrol was isolated by acid extraction employing a&nbsp;mixture hydrochloric acid-acetonitrile at 95&deg;C for 30 min followed by solid phase extraction. Relative standard deviations of reproducibility and repeatability were 1.77% and 5.49%, respectively. Spiking recovery value of 92% was achieved. Alfalfa, variety Morava, contains 148&ndash;248 mg.kg<sup>&ndash;1</sup>&nbsp;coumestrol in dry matter. The proposed method is useful for routine analyses.

Residue Analysis of Organophosphorus and Organochlorine Pesticides in Fatty Matrices by Gas Chromatography Coupled with Electron-Capture Detection

2006 ◽  
Vol 61 (5-6) ◽  
pp. 341-346 ◽  
Author(s):  
Jae-Woo Park ◽  
A. M. Abd El-Aty ◽  
Myoung-Heon Lee ◽  
Sung-Ok Song ◽  
Jae-Han Shim
Keyword(s):  
Gas Chromatography ◽  
Electron Capture ◽  
Simple Procedure ◽  
Linear Regression Analysis ◽  
Residue Analysis ◽  
Electron Capture Detection ◽  
Relative Standard ◽  
Wide Range ◽  
Repeatability And Reproducibility

A multiresidue method for the simultaneous determination of 22 organochlorine (OCs) and organophosphorus (Ops) pesticides (including isomers and metabolites), representing a wide range of physicochemical properties, was developed in fatty matrices extracted from meat. Pesticides were extracted from samples with acetonitrile/n-hexane (v :v, 1:1). The analytical screening was performed by gas chromatography coupled with electron-capture detection (ECD). The identification of compounds was based on their retention time and on comparison of the primary and secondary ions. The optimized method was validated by determining accuracy (recovery percentages), precision (repeatability and reproducibility), and sensitivity (detection and quantitation limits) from analyses of samples fortified at 38 to 300 ng/g levels. Correlation coefficients for the 22 extracted pesticide standard curves (linear regression analysis, n = 3) ranged from 0.998 to 1.000. Recovery studies from 2 g samples fortified at 3 levels demonstrated that the GC-ECD method provides 64.4-96.0% recovery for all pesticides except 2,4′-DDE (44.6-50.4%), 4,4′-DDE (51.1-57.5%) and 2,4′-DDT (50.0-51.2%). Both repeatability and reproducibility relative standard deviation values were < 20% for all residues. Detection limits ranged from 0.31 to 1.27 ng/g and quantification limits were between 1.04 and 4.25 ng/g. The proposed analytical method may be used as a simple procedure in routine determinations of OCs and Ops in meat. It can also be applied to the determination of pesticide multi-residues in other animal products such as butter and milk.

scholarly journals Determination of Chlorinated Phenols in Water and Soil by Capillary Zone Electrophoresis

1997 ◽  
Vol 80 (6) ◽  
pp. 1308-1314 ◽  
Author(s):  
Wayne E Rae ◽  
Charles A Lucy
Keyword(s):  
Capillary Zone Electrophoresis ◽  
Fused Silica ◽  
Soil Samples ◽  
Chlorinated Phenols ◽  
Relative Standard ◽  
Zone Electrophoresis ◽  
Water And Soil Samples ◽  
Fused Silica Capillary ◽  
Capillary Zone

Abstract A capillary zone electrophoresis (CZE) method was developed to separate and determine chlorinated phenols in water and soil samples. A mixture of 16 chlorinated phenols was resolved in 25 min by using a 77 cm (70 cm to detector) × 75 μm fused silica capillary with 0.015M tetraborate/0.045M phosphate (pH 7.3) buffer at 22 kV. Calibration linearities for water samples in the low parts-permillion range were good (correlation coefficient &gt; 0.99) for all solutes except p-chlorophenol. Average precision was 17% relative standard deviation. Typical detection limits were in the 200 μg/L range. Recoveries of chlorinated phenols from synthetic soil samples with methanol were quantitative.

Surrogate-Assisted Determination of 2,3,7,8-Tetrachlorodibenzo-p-Dioxin in Fish by Electron Capture Capillary Gas Chromatography

1986 ◽  
Vol 69 (6) ◽  
pp. 976-980
Author(s):  
Richard A Niemann
Keyword(s):  
Gas Chromatography ◽  
Electron Capture ◽  
Capillary Gas Chromatography ◽  
Capillary Column ◽  
Electron Capture Detection ◽  
Matrix Interference ◽  
Relative Standard ◽  
Tetrachlorodibenzo P Dioxin ◽  
Liquid Chromatographic

Abstract Surrogate spiking the sample with 1000 parts per trillion (pptr) 1,3,7,8-tetrachlorodibenzo-p-dioxin (1378-TCDD) has doubled analytical throughput in determining toxic 2378-TCDD (analyte) at the low partper- trillion level in fish, using multicolumn high resolution liquid chromatographic cleanup before quantitation by capillary gas chromatography with electron capture detection. The 1378- and 2378-TCDD were recovered equally and were well separated by the capillary column so that the earlier-eluting surrogate did not interfere with the quantitation of levels of analyte many-fold lower. Matrix interference contributed &lt;1 % bias in surrogate quantitation. Using surrogate recovery to correct for analyte losses during analysis, accuracy averaged (n = 7) 105% in determining 18 or 45 pptr 2378-TCDD added to fish without detectable bioincurred analyte. Analyses of selected fish with bioincurred 2378-TCDD gave results comparable to earlier work where recovery correction required a second analysis of sample fortified with analyte. With surrogate fortification, repeatability of determination (n = 3 or 4) improved markedly to &lt;5% relative standard deviation at 37-46 pptr.

scholarly journals Simultaneous Determination of Benzene and Toluene in Pesticide Emulsifiable Concentrate by Headspace GC-MS

2013 ◽  
Vol 2013 ◽  
pp. 1-5 ◽  
Author(s):  
Lidong Cao ◽  
Hua Jiang ◽  
Jing Yang ◽  
Li Fan ◽  
Fengmin Li ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Internal Standard ◽  
Fused Silica ◽  
Gas Chromatography Mass Spectrometry ◽  
Equilibration Time ◽  
Emulsifiable Concentrate ◽  
Pesticide Formulations ◽  
Relative Standard ◽  
Standard Additions

The toxic inert ingredients in pesticide formulations are strictly regulated in many countries. In this paper, a simple and efficient headspace-gas chromatography-mass spectrometry (HSGC-MS) method using fluorobenzene as an internal standard (IS) for rapid simultaneous determination of benzene and toluene in pesticide emulsifiable concentrate (EC) was established. The headspace and GC-MS conditions were investigated and developed. A nonpolar fused silica Rtx-5 capillary column (30 m×0.20 mmi.d. and 0.25 μm film thickness) with temperature programming was used. Under optimized headspace conditions, equilibration temperature of 120°C, equilibration time of 5 min, and sample size of 50 μL, the regression of the peak area ratios of benzene and toluene to IS on the concentrations of analytes fitted a linear relationship well at the concentration levels ranging from 3.2 g/L to 16.0 g/L. Standard additions of benzene and toluene to blank different matrix solutions 1ead to recoveries of 100.1%–109.5% with a relative standard deviation (RSD) of 0.3%–8.1%. The method presented here stands out as simple and easily applicable, which provides a way for the determination of toxic volatile adjuvant in liquid pesticide formulations.

Sign in / Sign up

Export Citation Format

Share Document