Determination of δ-hexadecansultone in sodium α-olefinesulphonates and liquid detergents using gas chromatography-mass spectrometry (GC/MS)

2019 ◽  
Vol 85 (7) ◽  
pp. 16-21
Author(s):  
Liliya R. Mubarakova ◽  
German K. Budnikov
Keyword(s):  
Multicomponent Mixture ◽  
Operating Mode ◽  
Complete Separation ◽  
Gas Chromatography Mass Spectrometry ◽  
Liquid Detergent ◽  
Cyclic Esters ◽  
Alcohol Water ◽  
Household Chemicals ◽  
Hydrolysis Of

Sultones are cyclic esters of hydroxysulfonic acids, which are formed in the process of sulfonation of α-olefins with sulfur trioxide gas. More stable sultones may be present in the final product — an anionic surfactant — sodium α-olefin sulfonate (AOC-Na). AOC-Na is widely used in the production of household chemicals and cosmetic products, including liquid dishwashing detergents. Sultones are strong skin sensitizers, their level in AOC-Na should be strictly controlled and not exceed 5 ppm. Operational and strict control of the sultone content upon AOC-Na production allows timely adjustment at the stage of hydrolysis, which leads to a more complete disclosure of the sultone cycle with the formation of the corresponding olefin sulfonates and hydroxyalkanesulfonates. We propose a method for determining δ-hexadecansultone in liquid dishwashing detergents and sodium α-olefinsulfonates obtained on the basis of α-olefins of C14 – C16 fractions using GC/MS, which provides shortening of sample preparation and keeps the sensitivity with a detection limit of 0.02 mg/kg. The effect of various weakly polar and non-polar organic solvents used for Sultone extraction from AOC-Na and liquid detergent on liquid extraction based on the dispersion of the extractant in an alcohol/water phase is studied. When selecting the solvent we have shown that the use of diethyl ether provided the best extraction of the analyte. Determination of the analyte extraction recovery was performed using the reaction of hydrolysis of the extracted mixture. We specified the operating mode of the device which provided complete separation of the components of the analyzed compounds including the samples of liquid detergent for dishes being a multicomponent mixture of complex composition.

Determination of Pesticides in Indoor Air and Dust

1993 ◽  
Vol 76 (5) ◽  
pp. 1121-1126 ◽  
Author(s):  
Kurt S Roinestad ◽  
Judith B Louis ◽  
Joseph D Rosen
Keyword(s):  
Indoor Air ◽  
Pesticide Exposure ◽  
Ion Trap ◽  
Gas Chromatography Mass Spectrometry ◽  
Simple Method ◽  
Limits Of Detection ◽  
Ion Trap Mass Spectrometer ◽  
Household Chemicals ◽  
Multiresidue Determination

Abstract Improved analytical and sampling methods were developed for the multiresidue determination of pesticides in indoor air. Air analysis consists of adsorption of the pesticides in 1 m3 of air onto Tenax TA via an air sampling pump, desorption with acetone, and determination and quantitation by gas chromatography/mass spectrometry (GC/MS) with chemical ionization on an ion trap mass spectrometer. Limits of detection for the 23 pesticides studied ranged from 0.5 ng/m3 for chlorpyrifos and diazinon to 30 ng/m3 for o-phenylphenol (approximately 0.5-30 parts per trillion on a w/w basis). A simple method for the detection of pesticides in dust was also developed. This method involves emptying the contents of a vacuum cleaner bag into a standard household food processor and extracting 1 g homogenized dust with acetone before GC/MS. Limits of detection were 25-100 ppb because of interferences by common household chemicals. However, pesticide concentrations were higher in dust than in air, therefore, analysis of dust is a better indicator of indoor pesticide exposure.

scholarly journals Contamination of pine and birch wood dust with microscopic fungi and determination of its sterol contents

2017 ◽  
Vol 68 (2) ◽  
pp. 127-134
Author(s):  
Kinga Stuper-Szablewska ◽  
Tomasz Rogoziński ◽  
Juliusz Perkowski
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Ultra Performance Liquid Chromatography ◽  
Complete Separation ◽  
Gas Chromatography Mass Spectrometry ◽  
Wood Dust ◽  
Chemical Analyses ◽  
Birch Wood ◽  
Microscopic Fungi

Abstract Wood compounds, especially sterols, are connected with the level of contamination with microscopic fungi. Within this study, tests were conducted on wood dust samples collected at various work stations in a pine and birch timber conversion plant. Their contamination with mycobiota was measured as the concentration of ergosterol (ERG) by ultra performance liquid chromatography (UPLC). Another aim of this study was to assess the effect of contamination with microscopic fungi on the sterol contents in wood dusts. Analyses were conducted on five sterols: desmosterol, cholesterol, lanosterol, stigmasterol, and β-sitosterol using UPLC and their presence was confirmed using gas chromatography/mass spectrometry (GC/MS). The results of chemical analyses showed the greatest contamination with mycobiota in birch wood dust. We also observed varied contents of individual sterols depending on the wood dust type. Their highest concentration was detected in birch dust. The discriminant analysis covering all tested compounds as predictors showed complete separation of all tested wood dust types. The greatest discriminatory power was found for stigmasterol, desmosterol, and ergosterol.

scholarly journals A New Gas Chromatography–Mass Spectrometry Method for Simultaneous Determination of Total and Free trans-3′-Hydroxycotinine and Cotinine in the Urine of Subjects Receiving Transdermal Nicotine

1999 ◽  
Vol 45 (1) ◽  
pp. 85-91 ◽  
Author(s):  
Allena J Ji ◽  
George M Lawson ◽  
Rodger Anderson ◽  
Lowell C Dale ◽  
Ivana T Croghan ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Simultaneous Determination ◽  
Gas Chromatography Mass Spectrometry ◽  
Chromatography Mass Spectrometry ◽  
Transdermal Nicotine ◽  
Selective Ion Monitoring ◽  
Lower Limits ◽  
Hydrolysis Of

Abstract trans-3′-Hydroxycotinine (THOC) has been recognized as the most abundant metabolite of nicotine. In an attempt to assess THOC and cotinine (COT) concentrations during nicotine transdermal therapy, we developed a new quantitative gas chromatography–mass spectrometry (GC–MS) method for simultaneous determination of total and free THOC and COT in human urine. The method utilizes the following: (a) hydrolysis of conjugated THOC and COT by β-glucuronidase; (b) basic extraction of THOC and COT with mixed dichloromethane and n-butyl acetate; (c) derivatization of THOC with bis(trimethylflurosilyl)acetamide; and (d) separation and identification by GC–MS with selective ion monitoring. Lower limits of quantification for the assay were 50 and 20 μg/L for THOC and COT, respectively. The intra- and interassay CVs were 4.4% and 11% for THOC, and 3.9% and 10% for COT at 1000 μg/L. The results from six consecutive 24-h urine collections in 71 subjects administered daily transdermal nicotine doses of 11, 22, and 44 mg showed that, on average, free THOC was 76% of total THOC and free COT was 48% of total COT in all subjects. THOC is the major metabolite of nicotine and constitutes 20% of total nicotine intake at steady state, whereas urinary nicotine and COT excretion were 8% and 17%, respectively. The method is useful for simultaneous determination of free and total THOCand COT and can be used to assess the urinary excretion of these metabolites during transdermal nicotine therapy.

scholarly journals Determination of natural and synthetic oestrogens in surface water using gas chromatography-mass spectrometry

2014 ◽  
Vol 58 (4) ◽  
pp. 603-611 ◽  
Author(s):  
Barbara Woźniak ◽  
Alicja Kłopot ◽  
Iwona Matraszek-Żuchowska ◽  
Katarzyna Sielska ◽  
Jan Żmudzki
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Surface Water ◽  
Capillary Column ◽  
Gas Chromatography Mass Spectrometry ◽  
Detection Capability ◽  
Chromatography Method ◽  
Rivers And Lakes ◽  
Hydrolysis Of

Abstract A simple and sensitive gas chromatography method was developed to determine a group of oestrogens in surface water. In the first stage of analysis, enzymatic hydrolysis of oestrogen metabolites with glucuronidase AS-HP was performed. Free compounds were extracted from 200 mL of water sample on C18 SPE column (6 mL, 1000 mg). The evaporated extract was subjected to derivatisation with a mixture of MSTFA/NH4I/DTT (1000:2:5, v/w/w). The separation of the analytes on HP-5ms capillary column was conducted. The method was validated according to the Commission Decision 2002/657/EC. Recovery in spiked samples ranged from 90% to 120 % with standard deviation lower than 30% for all examined compounds. The decision limit and detection capability of five oestrogens were in the range of 0.3-0.6 ng L-1 and 0.5-0.9 ng L-1, respectively. Nineteen water samples collected from different sites of several Polish rivers and lakes were tested for the presence of oestrogens. Some target compounds such as 17α-oestradiol, 17β-oestradiol, oestrone, oestriol, and 17α-ethynyloestradiol were found in trace amounts in the analysed samples. The highest concentration observed for oestradiol reached 23 ng L-1.

scholarly journals Simultaneous identification and quantitation of codeine, morphine, hydrocodone, and hydromorphone in urine as trimethylsilyl and oxime derivatives by gas chromatography–mass spectrometry

1997 ◽  
Vol 43 (6) ◽  
pp. 1029-1032 ◽  
Author(s):  
Larry A Broussard ◽  
Lance C Presley ◽  
Thomas Pittman ◽  
Randy Clouette ◽  
Gary H Wimbish
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Solid Phase ◽  
Gas Chromatography Mass Spectrometry ◽  
Selected Ion Monitoring ◽  
Chromatography Mass Spectrometry ◽  
Oxime Derivatives ◽  
Simultaneous Identification ◽  
Hydrolysis Of

Abstract Following enzymatic hydrolysis of urine, a gas chromatography–mass spectrometry method for the simultaneous determination of codeine, morphine, hydrocodone, and hydromorphone uses hydroxylamine to form oxime derivatives of the keto-opiates (i.e., hydrocodone, hydromorphone, oxycodone, and oxymorphone). These trimethylsilyl-derivatized forms no longer interfere with the detection and quantitation of codeine and morphine. Samples are extracted on solid-phase columns and quantitated by deuterated internal calibrations of each analyte with selected ion monitoring. Codeine, morphine, hydrocodone, and hydromorphone are completely separated, allowing simultaneous quantitation without interference and a chromatographic analysis time <9 min.

Determination of 2-Ethyl-l-Hexanol as Contaminant in Drinking Water

1993 ◽  
Vol 76 (5) ◽  
pp. 1133-1137 ◽  
Author(s):  
M Vitali ◽  
V Leoni ◽  
S Chiavarini ◽  
C Cremisini
Keyword(s):  
Gas Chromatography ◽  
Drinking Water ◽  
Analytical Procedure ◽  
Gas Chromatography Mass Spectrometry ◽  
Flame Ionization ◽  
Organoleptic Characteristics ◽  
Acidic Conditions ◽  
Ethylhexyl Phthalate ◽  
Hydrolysis Of

Abstract An analytical procedure for the determination of 2-ethyl-1-hexanol (2-EH) in drinking water is presented. The method is based on volatile-compound stripping, adsorption on activated-charcoal-filled tubes, solvent elution, identification by gas chromatography/ mass spectrometry, and determination by gas chromatography with flame ionization detection. Bottled samples with undesirable organoleptic characteristics were analzyed to determine a possible correlation with the presence of 2-EH. The presence of 2-EH at 2-10 μg/L was confirmed in several samples. The presence of di-2-ethylhexyl phthalate (D2EHP) was also checked in all samples. This compound was always found at 2-30 μg/L. Hydrolysis of D2EHP was carried out for 2 weeks to evaluate its possible contribution to water contamination by 2-EH. Tests did not show measurable amounts of the alcohol. Nonetheless, the hydrolysis of phthalates in the weakly acidic conditions of the examined waters would not justify the presence of 2-EH at the observed levels, and so it is reasonable to hypothesize a direct contamination from packaging materials containing 2-EH as residue from D2EHP synthesis.

DETERMINATION OF MICRO-AMOUNTS OF 5β-PREGNAN-3α-OL-20-ONE IN URINE USING INFRARED-SPECTROMETRY

1962 ◽  
Vol 41 (2) ◽  
pp. 234-246 ◽  
Author(s):  
H. J. van der Molen
Keyword(s):  
Infrared Spectrum ◽  
Quantitative Determination ◽  
Acid Hydrolysis ◽  
Chromatographic Separation ◽  
Pure Form ◽  
Infrared Spectrometry ◽  
Hydrolysis Of

ABSTRACT A procedure for the quantitative determination of 5β-pregnan-3α-ol-20-one in urine is described. After acid hydrolysis of the pregnanolone-conjugates in urine, the free steroids are extracted with toluene. Pregnanolone is isolated in a pure form as its acetate; after chromatographic separation of the free steroids on alumina, the fraction containing pregnanolone is acetylated and rechromatographed on alumina. Quantitative determination of the isolated pregnanolone-acetate is carried out with the aid of the infrared spectrum recorded by a micro KBr-wafermethod. The reliability of the method under various conditions is discussed under the headings, specificity, accuracy, precision and sensitivity. It is possible to determine 30–40 μg pregnanolone in a 24-hours urine portion with a precision of 25%.

EINE CHEMISCHE METHODE ZUR BESTIMMUNG VON 16-EPI-ÖSTRIOL IM URIN DES MENSCHEN

1963 ◽  
Vol 44 (1) ◽  
pp. 47-66 ◽  
Author(s):  
W. Nocke ◽  
H. Breuer
Keyword(s):  
Melting Point ◽  
Phosphoric Acid ◽  
Aqueous Alkali ◽  
Percentage Error ◽  
Organic Layer ◽  
Maximum Percentage ◽  
Chemical Determination ◽  
Routine Assay ◽  
Hydrolysis Of

ABSTRACT A method for the chemical determination of 16-epi-oestriol in the urine of nonpregnant women with a qualitative sensitivity of less than 0.5 μg/24 h is described. The separation of 16-epi-oestriol and oestriol is accomplished by converting 16-epi-oestriol into its acetonide, a reaction which is stereoselective for cis-glycols and therefore not undergone by oestriol as a trans-glycol. Following partition between chloroform and aqueous alkali, the acetonide of 16-epi-oestriol is completely separated with the organic layer whereas oestriol as a strong phenol remains in the alkaline phase. 16-epi-oestriol is chromatographed on alumina as the acetonide and determined as a Kober chromogen. This procedure can easily be incorporated into the method of Brown et al. (1957 b) thus making possible the simultaneous routine assay of oestradiol-17β, oestrone, oestriol and 16-epi-oestriol from one sample of urine. The specificity of the method was established by separation of 16-epi-oestriol from nonpregnancy urine as the acetonide, hydrolysis of the acetonide by phosphoric acid, isolation of the free compound by microsublimation and identification by micro melting point, colour reactions and chromatography. The accuracy of the method is given by a mean recovery of 64% for pure crystalline 16-epi-oestriol when added to hydrolysed urine in 5–10 μg amounts. The precision is given by s = 0.24 μg/24 h. For the duplicate determination of 16-epi-oestriol the qualitative sensitivity is 0.44 μg/24 h, the maximum percentage error being ± 100% The quantitative sensitivity (±25% error) is 1.7 μg/24 h.

INDIREKTE PAPIERCHROMATOGRAPHISCHE METHODE ZUR BESTIMMUNG DER HARNOESTROGENE

1961 ◽  
Vol 38 (4) ◽  
pp. 545-562 ◽  
Author(s):  
L. Kecskés ◽  
F. Mutschler ◽  
I. Glós ◽  
E. Thán ◽  
I. Farkas ◽  
...  
Keyword(s):  
Pregnant Women ◽  
Granulosa Cell ◽  
Iron Content ◽  
List Type ◽  
Granulosa Cell Tumour ◽  
Hydrolysis Of ◽  
Phenol Fraction ◽  
Qualitative Determination

ABSTRACT 1. An indirect paperchromatographic method is described for separating urinary oestrogens; this consists of the following steps: acidic hydrolysis, extraction with ether, dissociation of phenol-fractions with partition between the solvents. Previous purification of phenol fraction with the aid of paperchromatography. The elution of oestrogen containing fractions is followed by acetylation. Oestrogen acetate is isolated by re-chromatography. The chromatogram was developed after hydrolysis of the oestrogens 'in situ' on the paper. The quantity of oestrogens was determined indirectly, by means of an iron-reaction, after the elution of the iron content of the oestrogen spot, which was developed by the Jellinek-reaction. 2. The method described above is satisfactory for determining urinary oestrogen, 17β-oestradiol and oestriol, but could include 16-epioestriol and other oestrogenic metabolites. 3. The sensitivity of the method is 1.3–1.6 μg/24 hours. 4. The quantitative and qualitative determination of urinary oestrogens with the above mentioned method was performed in 50 pregnant and 9 non pregnant women, and also in 2 patients with granulosa cell tumour.

Sign in / Sign up

Export Citation Format

Share Document