1,2-Propanediol Determination in working air with gas chromatography with mass spectrometer

2017 ◽  
Vol 33 (2(92)) ◽  
pp. 173-188
Author(s):  
Wiktor Wesołowski ◽  
MAŁGORZATA KUCHARSKA
Keyword(s):  
Propylene Glycol ◽  
Electronic Cigarettes ◽  
Mass Detection ◽  
Limit Of Quantification ◽  
Chromatographic Separations ◽  
Polyester Resins ◽  
Selective Determination ◽  
Workplace Air ◽  
Main Component

Propane-1,2-diol (propylene glycol, PG) is a color-less, strongly hygroscopic liquid used in the pro-duction of antifreeze fluids, polyester resins and detergents. The main use of propane-1,2-diol is in the cosmetic industry as an ingredient of creams, toothpastes, mouthwashes and deodorant sticks. It is also used in medicine, pharmaceutics, food and cleaning products. Propane-1,2-diol is used as a hygroscopic agent in the plastics industry, textile products and in manufacturing cigarettes. Recently, it is used as the main component of fluids used in electronic cigarettes. There are no reports in the literature on acute poi-soning with propylene glycol of people in occupa-tional exposure conditions. Clinical observations of people treated with propylene glycol applied as a drug solvent indicate a weak narcotic effect of the compound and mild irritation of the skin and con-junctives. The aim of this study was to develop and validate a sensitive method for determining concentrations of propane-1,2-diol in workplace air in the range from 1/20 to 2 MAC values in accordance with the requirements of Standard No. PN-EN 482+A1:2016-1. The study was performed using a gas chromatog-raphy (GC). A 6890N Agilent Technologies gas chromatograph with a 5973 mass spectrometry de-tector (MSD), HP-PONA (50 m; 0.2 mm; 0,5 μm) ca-pillary analytical column, autosampler and Chem-Station software were used for chromatographic separations. The method is based on the adsorption of inhalable fraction and vapors of propane-1,2-diol on glass fi-ber filters and XAD-7 resin, desorption with ace-tonitrile and analysis of the resulting solution with gas chromatographic with mass detection (GC/MS). The extraction efficiency of propane-1,2--diol from filters and resin was 97.3%. Samples of propane-1,2-diol can be stored in refrigerator for up to 28 days. Application of a HP-PONA capillary column enabled selective determination of pro-pane-1,2-diol in a mixture of acetonitrile, dichloro-methane, toluene and other compounds. The method is linear (r = 0.9992) within the work-ing range 10–500 μg/ml, which is equivalent to air concentrations range 4.4–222 mg/m3 for a 180-L air sample and 80-fold dilution. Limit of quantification (LOQ) is 1.303 μg/ml. The analytical method described in this paper ena-bles selective determination of inhalable fraction and vapors of propane-1,2-diol in workplace air in presence of other compounds at concentrations from 4.4 to 222 mg/m3 (1/20–2 MAC value). The method is precise, accurate and it meets the criteria for procedures for measuring chemical agents listed in Standard No. PN-EN 482+A1:2016-1. The method can be used for assessing occupational exposure to propane-1,2-diol and associated risk to workers’ health. The developed method of determining propane-1,2-diol has been recorded as analytical procedure (see appendix).

Chlorobenzene. Determination in workplace air

2019 ◽  
Vol 35 (1(99)) ◽  
pp. 19-28
Author(s):  
Anna Jeżewska ◽  
Agnieszka Woźnica
Keyword(s):  
Occupational Exposure ◽  
Carbon Disulfide ◽  
Limit Of Detection ◽  
Skin Irritation ◽  
Raw Material ◽  
Good Precision ◽  
Limit Of Quantification ◽  
Selective Determination ◽  
Workplace Air

Chlorobenzene is a colorless, flammable liquid that has an almond-like odor. It is used in industry as a solvent: resins, paints and fats, raw material for the production of plastics, as well as for the production of phenol, aniline and nitrobenzene. Occupational exposure to chlorobenzene vapors can occur through inhalation, absorption through the skin or ingestion. Harmful if inhaled, causes skin irritation. Long-term exposure affects the central nervous system. The aim of this study was an amendment to the PN-Z-04022- 03:2001 withdrawn from the Polish set of standards, and validate method for determination concentrations of chlorobenzene in the workplace air in the range from 1/10 to 2 MAC values, in accordance with the requirements of the standard PN-EN 482. The study was performed using a gas chromatograph (GC) with a flame ionization detector (FID) equipped with a capillary column HP-5 (30 m x 0.32 mm, 0.25 μm). This method is based on the adsorption of chlorobenzene vapors on activated charcoal, desorption with carbon disulfide, and analyzed by GC-FID. Application of HP-5 column allows selective determination of chlorobenzene in a presence of carbon disulfide, aniline, phenol and nitrobenzene. The measurement range was 2.3 ÷ 46 mg/m3 for a 15 l air sample. Limit of detection: 6.75 ng/ml and limit of quantification: 20.25 ng/ml. Analytical method described in this paper enables selective determination of chlorobenzene in workplace atmosphere in presence of other solvents at concentrations from 2.3 mg/m3 (1/10 MAC value). The method is characterized by good precision and accuracy and meets the criteria for the performance of procedures for the measurement of chemical agents, listed in EN 482. The method may be used for the assessment of occupational exposure to chlorobenzene and the associated risk to workers’ health. The developed method of determining chlorobenzene has been recorded as an analytical procedure (see Appendix). This article discusses the problems of occupational safety and health, which are covered by health sciences and environmental engineering.

1,2-Dichloroethane. Determination in workplace air

2018 ◽  
Vol 34 (2(96)) ◽  
pp. 133-143
Author(s):  
Agnieszka Woźnica
Keyword(s):  
Limit Of Detection ◽  
Flammable Liquid ◽  
Limit Of Quantification ◽  
Selective Determination ◽  
Flame Ionization ◽  
Chemical Agents ◽  
Workplace Air ◽  
Other Substances ◽  
Air Sample

1,2-Dichloroethane is a colorless, highly flammable liquid with a chloroform-like odor. This substance is used in industry as an intermediate in the production of vinyl chloride, but it is also used in the production of other chlorinated hydrocarbons. It is also used as a solvent. 1,2-Dichloroethane is carcinogenic for humans. The aim of this study was to develop a method for determining concentrations of 1,2-dichloroethane in the workplace air in the range from 1/10 to 2 MAC values (0.82–16.4 mg/m3). The study was performed using a gas chromatograph (GC) with a flame ionization detector (FID) equipped with a capillary column HP-1 (50 m x 0.32 mm; 0.3 μm). The method is based on the adsorption of 1,2-dichloroethane on activated charcoal, desorption of analyzed compound with carbon disulfide and analysis of obtained solution with GC-FID. The use of HP-1 column enabled selective determination of 1,2-dichloroethane in a presence of other substances. The average desorption coefficient of 1,2-dichloroethane from charcoal was 0.98. The method is linear (r = 0.9999) within the investigated working range from 9.84 to 196.8 μg/ml, which is equivalent to air concentrations from 0.82 to 16.4 mg/m3 for a 12-L air sample. The limit of detection (LOD) and limit of quantification (LOQ) were to 2.284 μg/ml and 6.85 μg/ml, respectively. The analytical method described in this paper enables selective determination of 1,2-dichloroethane in workplace air in presence of other substances at concentrations from 0.82 mg/m3 (1/10 MAC value). The method is precise, accurate and it meets the criteria for procedures for measuring chemical agents listed in Standard No. EN 482. The method can be used for assessing occupational exposure to 1,2-dichloroethane and associated risk to workers’ health. The developed method of determining 1,2-dichloroethane has been recorded as an analytical procedure (see appendix).

But-2-enal. Determination in workplace air

2019 ◽  
Vol 35 (1(99)) ◽  
pp. 5-18
Author(s):  
Anna Jeżewska ◽  
Agnieszka Woźnica
Keyword(s):  
Limit Of Detection ◽  
Array Detector ◽  
Good Precision ◽  
European Standard ◽  
Limit Of Quantification ◽  
Liquid Chromatograph ◽  
Selective Determination ◽  
Validation Parameters ◽  
Workplace Air

But-2-enal (crotonaldehyde) is a colourless liquid with an unpleasant suffocating odour. But-2-enal occurs naturally in food. It is mainly used for the production of sorbic acid, a food preservative. But-2-enal is a very toxic, highly irritating and allergenic substance – it is suspected of causing genetic defects. The aim of the study was to develop a method for determination of but-2-enal, which will enable determination of concentrations of this substance in the workplace air in the range from 1/10 to 2 MAC values. The tests were performed using a liquid chromatograph (HPLC) with a diode array detector (DAD), equipped with an Ultra C18 column (250 x 4.6 mm; 5 μm). The method consists in retaining the but-2-enal on a silica gel coated with 2,4-dinitrophenylhydrazine. The sample is extracted with acetonitrile and analyzed by HPLC. Validation of the method was carried out in accordance with the requirements of the European standard EN 482. The measuring range of the method is from 0.1 to 2 mg/m3 for a 12 l sample of air. The following validation parameters were obtained: limit of detection: 1.26 ng/ml (0.21 μg/m3), limit of quantification: 3.77 ng/ml (0.63 μg/m3), the overall accuracy of the method: 5.08%, expanded uncertainty: 22%. The developed analytical method enables selective determination of but-2-enal in workplace air at concentrations ranging from 0.1 mg/m3, i.e. from 1/10 of the MAC value in the presence of co-occurring substances. The method is characterized by good precision and accuracy and meets the requirements of the European standard PN-EN 482 for procedures for determination of chemical agents. The developed method of determining but-2-enal has been recorded as an analytical procedure (see Appendix). This article discusses the problems of occupational safety and health, which are covered by health sciences and environmental engineering.

Dimethyl phthalate. Determination in workplace air

2019 ◽  
Vol 36 (2(100)) ◽  
pp. 47-59
Author(s):  
Agnieszka Woźnica
Keyword(s):  
Occupational Exposure ◽  
Occupational Safety ◽  
Limit Of Detection ◽  
Measurement Range ◽  
Good Precision ◽  
Dimethyl Phthalate ◽  
Limit Of Quantification ◽  
Selective Determination ◽  
Workplace Air

Dimethyl phthalate (DMP) is a colourless liquid with a slight aromatic odour. It is used in industry as a plasticizer of plastics, as an ingredient of fragrances in the production of cosmetics and detergents. Occupational exposure to DMP can occur through inhalation, or ingestion. The aim of this study was to validate a method for determining DMP concentration in workplace air in the range from 1/10 to 2 MAC values, in accordance with the requirements of standard PN-EN 482. The study was performed using a gas chromatograph (GC) with a flame ionization detector (FID) equipped with a capillary column HP-INNOWAX (60 m x 0.25 mm, 0.15 µm). This method is based on the sorption of dimethyl phthalate vapours on a glass microfiber filter, desorption with ethanol, and analyzed by GC-FID. The average desorption efficiency of DMP from filter was 98%. Application of HP-INNOWAX column allows selective determination of DMP in the presence of other solvents. The measurement range was 0.5 – 10 mg/m3 for a 120-L air sample. Limit of detection: 0.02 µg/ml and limit of quantification: 0.06 µg/ml. The analytical method described in this paper enables a selective determination of DMP in workplace air in the presence of other solvents at concentrations from 0.5 mg/m3 (1/10 MAC value). The method is characterized by good precision and accuracy and meets the criteria for the performance of procedures for the measurement of chemical agents, listed in EN 482. The method may be used for the assessment of occupational exposure to DMP and the associated risk to workers’ health. The developed method of determining DMP has been recorded as an analytical procedure (see appendix). This article discusses the problems of occupational safety and health, which are covered by health sciences and environmental engineering.

Diethyl phthalate Determination in workplace air

2017 ◽  
Vol 33 (1(91)) ◽  
pp. 127-137
Author(s):  
Agnieszka Woźnica
Keyword(s):  
Food Packaging ◽  
Limit Of Detection ◽  
Measurement Range ◽  
Diethyl Phthalate ◽  
Limit Of Quantification ◽  
Selective Determination ◽  
Nail Polish ◽  
Workplace Air ◽  
Other Substances

Diethyl phthalate (DEP) is an ester of phthalic acid and an ethanol. It is a colorless, oily liquid. This substance is used in industry as a solvent for cellulose acetate and nitrocellulose, and a plasticizer of plastics. It is added to nail polish, perfumes in cosmetics and detergents, food packaging and pharmaceuticals. Diethyl phthalate is a substance which is toxic if inhaled, irritating to eyes and skin, toxic for reproduction (it is suspected that acts harmful to fertility or unborn child). The aim of this study was to develop and validate a method for determining concentrations of diethyl phthalate in workplace air in the range from 1/10 to 2 MAC values in accordance with the requirements of Standard No. PN-EN 482. The study was performed using a gas chromatograph (GC) with a flame ionization detector (FID) with a capillary column HP-INNOWAX (60 m × 0.25 mm, 0.15 µm). The method is based on the adsorption of diethyl phthalate on glass microfiber filter, desorption of analysed compound with ethanol and analysis of the resulting solution with GC-FID. The average desorption efficiency of diethyl phthalate from filter was 90%. Application of column HP-INNOWAX enables selective determination of diethyl phthalate in the presence of other solvents. The measurement range was 0.3  6 mg/m3 for a 240-L air sample. The limit of detection (LOD) and the limit of quantification (LOQ) are 0.09 µg/ml and 0.27 µg/ml, respectively. The analytical method described in this paper enables selective determination of inhalable fraction of diethyl phthalate in workplace air in the presence of other substances at concentrations from 0.3 mg/m3 (1/10 MAC value). The method is precise, accurate and it meets the criteria for procedures for measuring chemical agents listed in Standard No. EN 482. The method can be used for assessing occupational exposure to diethyl phthalate and associated risk to workers’ health. The developed method of determining diethyl phthalate has been recorded as an analytical procedure (see appendix).

scholarly journals Fabrication of Efficient and Selective Modified Graphene Paste Sensor for the Determination of Catechol and Hydroquinone

Surfaces ◽  
2020 ◽  
Vol 3 (3) ◽  
pp. 473-483
Author(s):  
Jamballi G. Manjunatha
Keyword(s):  
Modified Electrode ◽  
High Sensitivity ◽  
Differential Pulse ◽  
Official Method ◽  
Limit Of Quantification ◽  
Selective Determination ◽  
Graphene Paste Electrode ◽  
Modified Graphene ◽  
Paste Electrode

An electrochemical sensor, based on a graphene paste electrode (GPE), was modified with a polymerization method, and the electrochemical behavior of catechol (CC) and hydroquinone (HQ) was investigated using electroanalytical methods like cyclic voltammetry (CV) and differential pulse voltammetry (DPV). The effect of CC at the modified electrode was evidenced by the positive shift of the oxidation peak potential of CC at the poly (rosaniline)-modified graphene paste electrode (PRAMGPE) and the nine-fold enhancement of the peak current, as compared to a bare graphene paste electrode (BGPE). The sensitivity of CC investigated by DPV was more sensitive than CV for the analysis of CC. The DPV method showed the two linear ranges of 2.0 × 10−6–1.0 × 10−5 M and 1.5 × 10−5–5 × 10−5 M. The detection limit and limit of quantification were determined to be 8.2 × 10−7 and 27.6 × 10−7 M, respectively. The obtained results were compared successfully with respect to those obtained using the official method. Moreover, this sensor is applied for the selective determination of CC in the presence of HQ. The high sensitivity, good reproducibility, and wide linear range make the modified electrode suitable for the determination of CC in real samples. The practical application of the sensor was demonstrated by determining the concentration of CC in water samples with acceptable recoveries (97.5–98%).

scholarly journals Determination of Propane-1,3-sultone in Workplace Air for Occupational Exposure Assessment

2020 ◽  
Vol 17 (4) ◽  
pp. 1414
Author(s):  
Anna Jeżewska
Keyword(s):  
Occupational Exposure ◽  
Limit Of Detection ◽  
Glass Tube ◽  
Gas Chromatograph ◽  
Measuring Range ◽  
Limit Of Quantification ◽  
Occupational Exposure Assessment ◽  
Workplace Air ◽  
Air Sample

Propane-1,3-sultone (PS) is an alkylating substance used in the production of polymers, fungicides, insecticides, dyes, and detergents. It is absorbed into the human body by inhalation, digestion, and through the skin; it is also a possible carcinogen. Occupational exposure to this substance may occur on industrial or laboratory contact. In Poland, the maximum allowable concentration (MAC) for PS in workplace air is 7 µg/m3. The paper presents a method for determination of PS in workplace air using a gas chromatograph coupled with a mass spectrometer (GC-MS). Air containing PS is passed through a glass tube containing a glass fiber filter and two layers of silica gel. The substance is washed with acetonitrile and the solution obtained analysed using GC-MS. The measuring range for an air sample of 360 L is 0.7 ÷ 14 µg/m3. The limit of detection (LOD) is 13 ng/m3, limit of quantification (LOQ) is 40 ng/m3.

Determination of ephedrine, pseudoephedrine, sinapine thiocyanate, tetrahydropalmatine and amygdalin by HPLC-MS/MS after oral administration of extracts of Majie cataplasm in rabbits plasma: Application to a pharmacokinetic study

2020 ◽  
Author(s):  
Changxiang Li ◽  
Hanfen Shi ◽  
Fafeng Cheng ◽  
Wenxiang Zhu ◽  
Yuanjun Liu ◽  
...  
Keyword(s):  
Oral Administration ◽  
Pharmacokinetic Study ◽  
Multiple Reaction Monitoring ◽  
Gradient Elution ◽  
Limit Of Quantification ◽  
Chromatographic Separations ◽  
Qualitative Detection ◽  
Chromatographic Resolution ◽  
First Time

Abstract BackgroundThis study aimed to develop HPLC-MS/MS method for quantification of ephedrine, pseudoephedrine, sinapine thiocyanate, tetrahydropalmatine and amygdalin of extracts of Majie cataplasm after oral administration in rabbits plasma and describe the pharmacokinetics of this five components.MethodsThe qualitative detection of the five compounds was accomplished by two methods. One method for the simultaneous determination of ephedrine, pseudoephedrine, sinapine thiocyanate and tetrahydropalmatine was developed and validated for the first time, while the other method was for amygdalin. Chromatographic separations were achieved on a C18 column using gradient elution with the mobile phase consisting of acetonitrile and water (containing 0.1% formic acid and 5mM ammonium formate) for ephedrine, pseudoephedrine, sinapine thiocyanate and tetrahydropalmatine, while acetonitrile and water for amygdalin, at a flow rate of 0.4 mL/min. The initial gradient was extended in order to isolate ephedrine and pseudoephedrine better. The detection was performed in multiple-reaction monitoring (MRM) mode using electrospray ionization (ESI).ResultsAll calibration curves showed good linearity (r2＞0.996) within the test ranges. The lower limit of quantification was 0.01 ng/mL for all five analytes. Reproducibility for five analytes ranged from 0.79 to 2.3% (Ephedrine), 0.51 to 3.4% (pseudoephedrine), 2.8 to 5.0% (Sinapine thiocyanate), 2.6 to 6.3% (Tetrahydropalmatine) and 1.1—2.5% (amygdalin) respectively. The extraction recoveries were within the acceptable range.ConclusionThe two methods were successfully applied to pharmacokinetic study of rabbits after oral administration. The two methods has several advantages including good chromatographic resolution, specific and reproducibility and superior minimum detection limit. The results provided a basis for further study on the bioactivity of Majie cataplasm.

2,2-Bis(4-hydroxyphenyl)propane – inhalation fraction. Determination method in workplace air

2017 ◽  
Vol 33 (3(93)) ◽  
pp. 141-150
Author(s):  
Marzena Bonczarowska ◽  
Sławomir Brzeźnicki
Keyword(s):  
Flame Retardants ◽  
Limit Of Detection ◽  
Upper Respiratory Tract ◽  
Negative Effects ◽  
Limit Of Quantification ◽  
Liquid Chromatograph ◽  
Selective Determination ◽  
Human Fertility ◽  
Workplace Air ◽  
Air Sample

2,2-Bis(4-hydroxyphenyl)propane (bisphenol A BPA) is a substance in a form of a solid crystals or flakes with a mild phenolic odor. BPA is commonly used in the production of epoxide, polycarbonate or polysulfone resins, glues, breaks fluids or as a flame retardants and fungicides. Exposure to BPA can cause irritation of skin, BPA can also act as a nefro or hepatotoxic factor and upper respiratory tract or mucous membranes of the eye. BPA has a negative effects on human fertility. The aim of this study was to develop and validate a sensitive method for determining BPA concentrations in workplace air in the range from 1/10 to 2 MAC values, in accordance with the requirements of Standard No. PN-EN 482. The study was performed using a liquid chromatograph with spectrophotometric (UV-VIS) and spectrofluorimetric (FLD) detection. All chromatographic analyses were performed with Supelcosil LC 18 (150 × 3 mm) analytical column, which was eluted with mixture of acetonitrile and water (1:1). This method was based on collecting BPA on glass fiber filter, extracting with acetonitrile, and chromatographic determining resulted solution with HPLC technique. The average extraction efficiency of BPA from filters was 90%. The method was linear (r = 0.9996) within the investigated working range 0.125–5 mg/m3 for a 720-L air sample. The calculated limit of detection (LOD) and the limit of quantification (LOQ) was to 0.02 μg/ml (UV-VIS) and 0.013 μg/ml (FLD), and 0.068 μg/ml (UV-VIS) and 0.042 μg/ml (FLD), respectively. The analytical method described in this paper enables specific and selective determination of BPA in workplace air in presence of other compounds. The method is precise, accurate and it meets the criteria for measuring chemical agents listed in Standard No. PN-EN 482+A1:2016-01. The method can be used for assessing occupational exposure to BPA and associated risk to workers’ health. The developed method of determining BPA has been recorded as an analytical procedure (see appendix).

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