Ethylenediamine. Determination in workplace air with high performance liquid chromatography – spectrophotometric technique

2019 ◽  
Vol 35 (1(99)) ◽  
pp. 61-76
Author(s):  
Marek Zieliński ◽  
Ewa Twardowska ◽  
Małgorzata Kucharska
Keyword(s):  
Occupational Exposure ◽  
Silica Gel ◽  
High Performance ◽  
Limit Of Detection ◽  
Acid Extraction ◽  
Upper Respiratory Tract ◽  
Limit Of Quantification ◽  
Liquid Chromatograph ◽  
Workplace Air

Ethylenediamine (EDA) is a colorless, viscous liquid with ammonia-like odor. It is used as an intermediate in manufacture of chelating agents (EDTA), fungicide, poliamide and formaldehyde-urea resins, surfactants, corrosion inhibitors, emulsifying agents and stabiliser of rubber products. EDA may cause irritation of upper respiratory tract, eye and skin. Occupational exposure to EDA may lead to alergic reactions and asthma. EDA is not classified as carcinogennic to humans. The aim of this study was to develop and validate a sensitive method for determining hydrazine concentrations in the 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 detection. All chromatographic analysis were performed with Supelcosil LC-18 (150 × 3 mm, 5 µm) analytical column, which was eluted with mixture of acetonitrile and water (6:4 v/v). The method is based on the collection of EDA on silica gel impregnated with sulfuric acid, extraction with mixture of acetonitrile and water (62:38 v/v), derivatization of extracted compound with 9-fluorenylmethyl chloroformate and chromatographic determination of resulted solution with HPLC technique. The method is linear (r = 0.9994) within the investigated working range 0.1–2 μg/ml (2–40 mg/m3 for a 10-L air sample). Calculated limit of detection (LOD) and limit of quantification (LOQ) were 0.04 μg/ml and 0.13 μg/ml, respectively. The average extraction efficiency of EDA from silica gel was 86% and samples stored in refrigerator are stable for 10 days. The analytical method described in this paper enables determination of EDA in workplace air. The method is precise, accurate and it meets the criteria for procedures for measuring chemical agents listed in Standard No. PN-EN 482. The method can be used for assessing occupational exposure to EDA and associated risk to workers’ health. The developed method of determining EDA 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.

Pentachlorophenol. Determination in workplace air by means of high performance liquid chromatography

2019 ◽  
Vol 35 (1(99)) ◽  
pp. 59-74
Author(s):  
Sławomir Brzeźnicki ◽  
Marzena Bonczarowska
Keyword(s):  
Occupational Exposure ◽  
Phosphoric Acid ◽  
Limit Of Detection ◽  
Crystalline Solid ◽  
Respiratory Disorder ◽  
Upper Respiratory Tract ◽  
Limit Of Quantification ◽  
Liquid Chromatograph ◽  
Workplace Air

Pentachlorophenol (PCF) in room temperature is a crystalline solid with phenol-like odor. It is soluble in most organic solvents (diethyl ether, acetone, carbon tetrachloride, methanol). It is slightly soluble in water. Pentachlorophenol is used as a fungicide, insecticide and as non-selective herbicide (defoliant) in cotton crops. It is also used as antimicrobial agent in leather, paper and textile industry. It has been widely used as wood preservative in wood and construction industry. Occupational exposure to pentachlorophenol may cause irritation of mucous membranes of the eyes and the upper respiratory tract and skin lesions. It may also lead to changes in the central nervous system like headache, insomnia, vertigo and depression. Acute poisoning may cause pulmonary edema, cardio-respiratory disorder and even death. Pentachlorophenol is also suspected to be carcinogenic to humans. The aim of this study was to develop and validate a sensitive method for determining pentachlorophenol 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 detection. All chromatographic analysis were performed with Zorbax SB-CN 250 × 4.6 mm analytical column, which was eluted with mixture of 0.1% phosphoric acid in acetonitrile and 0.1% phosphoric acid in water (6: 4 v/v). The method is based on the collection of pentachlorophenol on XAD 7 resin preceded by a glass fiber filter, extraction with methanol and chromatographic determination of resulted solution with HPLC technique. The method is linear (r = 0.9997) within the investigated working range 0.625–12.5 μg/ml (0.05–1.0 mg/m3 for a 25-L air sample). The calculated limit of detection (LOD) and limit of quantification (LOQ) were 0.014 μg/ml and 0.048 μg/ml, respectively. The average extraction efficiency of pentachlorophenol from filter and XAD 7 amounted to 95% and samples stored in refrigerator are stable for 14 days. The analytical method described in this paper enables determination of pentachlorophenol in workplace air. The method is precise, accurate and it meets the criteria for procedures for measuring chemical agents listed in Standard No. PN-EN 482. The method can be used for assessing occupational exposure to pentachlorophenol and associated risk to workers’ health. The developed method of determining pentachlorophenol 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.

Hydrazine. Determination in workplace air with high performance liquid chromatography – spectrophotometric technique

2019 ◽  
Vol 35 (1(99)) ◽  
pp. 45-57
Author(s):  
Marzena Bonczarowska ◽  
Patryk Piątek ◽  
Sławomir Brzeźnicki
Keyword(s):  
Limit Of Detection ◽  
Skin Irritation ◽  
International Agency ◽  
Dihydrogen Phosphate ◽  
Acid Extraction ◽  
Sodium Dihydrogen Phosphate ◽  
Limit Of Quantification ◽  
Liquid Chromatograph ◽  
Workplace Air

Anhydrous hydrazine in room temperature is colorless fuming oily liquid with ammonia-like odor. It is used in various industries for electrolytic plating of metals on glass and plastics, as a chemical intermediate for the synthesis of pesticides, insecticides, medicines and days. It is used also as water treatment agent in energy industry (corrosion inhibitor), rocket propellant and as explosives material. Long term exposure to hydrazine may cause to skin irritation and allergic reactions. Diluted aqueous solutions of hydrazine may be irritating for skin, eye and respiratory tract. Epidemiologic studies shows that chronic exposure to hydrazine may cause cancer. In European Union hydrazine is classified as a carcinogenic substance (cat. 1B). Experts from International Agency for Research on Cancer (IARC) have classified hydrazine as a compound probably carcinogenic to humans (Group 2A). Due to decreasing of MAC value for hydrazine in Poland it was necessary to develop and validate a sensitive method for determining hydrazine concentrations in the 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 detection. All chromatographic analysis were performed with Discovery LC-18 150 × 2,1 mm analytical column, which was eluted with mixture of acetonitrile and water (6:4 v/v). The method is based on the collection of hydrazine on glass fiber filter impregnated with sulfuric acid, extraction with mixture of sodium dihydrogen phosphate and EDTA, derivatization of extracted compound with benzaldehyde and chromatographic determination of resulted solution with HPLC technique. The method is linear (r = 0.9989) within the investigated working range 0.15–3.5 μg/ml (0.00125–0.029 mg/m3 for a 240-L air sample). Calculated limit of detection (LOD) and limit of quantification (LOQ) were 0.0007 μg/ml and 0.0023 μg/ml, respectively. The average extraction efficiency of hydrazine from filters was 97% and samples stored in refrigerator are stable for 14 days. The analytical method described in this paper enables determination of hydrazine in workplace air. The method is precise, accurate and it meets the criteria for procedures for measuring chemical agents listed in Standard No. PN-EN 482. The method can be used for assessing occupational exposure to hydrazine and associated risk to workers’ health. The developed method of determining hydrazine 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.

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.

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.

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).

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.

scholarly journals DETERMINATION OF 10-GINGEROL IN INDIAN GINGER BY VALIDATED HPTLC METHOD OF SAMPLES COLLECTED ACROSS SUBCONTINENT OF INDIA

2016 ◽  
Vol 8 (12) ◽  
pp. 190
Author(s):  
Kamran Ashraf ◽  
Syed Adnan Ali Shah ◽  
Mohd Mujeeb
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Aluminum Plates ◽  
Layer Chromatography ◽  
Hptlc Method

<p><strong>Objective: </strong>A simple, sensitive, precise, and accurate stability indicating HPTLC (high-performance thin-layer chromatography) method for analysis of 10-gingerol in ginger has been developed and validated as perICH guidelines.</p><p><strong>Methods: </strong>The separation was achieved on TLC (thin layer chromatography) aluminum plates pre-coated with silica gel 60F<sub>254</sub> using n-hexane: ethyl acetate 55:45 (%, v/v) as a mobile phase. Densitometric analysis was performed at 569 nm.</p><p><strong>Results: </strong>This system was found to have a compact spot of 10-gingerol at <em>R</em><sub>F</sub> value of 0.57±0.03. For the proposed procedure, linearity (<em>r</em><sup>2</sup> = 0.998±0.02), limit of detection (18ng/spot), limit of quantification (42 ng/spot), recovery (ranging from 98.35%–100.68%), were found to be satisfactory.</p><p><strong>Conclusion: </strong>Statistical analysis reveals that the content of 10-gingerol in different geographical region varied significantly. The highest and lowest concentration of 10-gingerol in ginger was found to be present in a sample of Patna, Lucknow and Surat respectively which inferred that the variety of ginger found in Patna, Lucknow are much superior to other regions of India.</p>

Determination of Potential Genotoxic Impurity, 5-Amino-2-Chloropyridine, in Active Pharmaceutical Ingredient Using the HPLC-UV System

2020 ◽  
Author(s):  
Murat Soyseven ◽  
Rüstem Keçili ◽  
Hassan Y Aboul-Enein ◽  
Göksel Arli
Keyword(s):  
Analytical Method ◽  
High Performance ◽  
Orthophosphoric Acid ◽  
Limit Of Detection ◽  
Detection System ◽  
Active Pharmaceutical Ingredient ◽  
Limit Of Quantification ◽  
Column Temperature ◽  
Water Ph

Abstract A novel analytical method, based on high-performance liquid chromatography with a UV (HPLC-UV) detection system for the sensitive detection of a genotoxic impurity (GTI) 5-amino-2-chloropyridine (5A2Cl) in a model active pharmaceutical ingredient (API) tenoxicam (TNX), has been developed and validated. The HPLC-UV method was used for the determination of GTI 5A2Cl in API TNX. The compounds were separated using a mobile phase composed of water (pH 3 adjusted with orthophosphoric acid): MeOH, (50:50: v/v) on a C18 column (150 × 4.6 mm i.d., 2.7 μm) at a flow rate of 0.7 mL min−1. Detection was carried out in the 254 nm wavelength. Column temperature was maintained at 40°C during the analyses and 10 μL volume was injected into the HPLC-UV system. The method was validated in the range of 1–40 μg mL−1. The obtained calibration curves for the GTI compound was found linear with equation, y = 40766x − 1125,6 (R2 = 0.999). The developed analytical method toward the target compounds was accurate, and the achieved limit of detection and limit of quantification values for the target compound 5A2Cl were 0.015 and 0.048 μg mL−1, respectively. The recovery values were calculated and found to be between 98.80 and 100.03%. The developed RP-HPLC-UV analytical method in this research is accurate, precise, rapid, simple and appropriate for the sensitive analysis of target GTI 5A2Cl in model API TNX.

Determination of tigecycline in turkey plasma by LC-MS/MS: validation and application in a pharmacokinetic study

2017 ◽  
Vol 20 (2) ◽  
pp. 241-249 ◽  
Author(s):  
A. Jasiecka-Mikołajczyk ◽  
J.J. Jaroszewski
Keyword(s):  
Pharmacokinetic Study ◽  
High Performance ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Reversed Phase ◽  
Selected Reaction Monitoring ◽  
Limit Of Quantification ◽  
Complicated Skin ◽  
Intravenous And Oral Administration

Abstract Tigecycline (TIG), a novel glycylcycline antibiotic, plays an important role in the management of complicated skin and intra-abdominal infections. The available data lack any description of a method for determination of TIG in avian plasma. In our study, a selective, accurate and reversed-phase high performance liquid chromatography-tandem mass spectrometry method was developed for the determination of TIG in turkey plasma. Sample preparation was based on protein precipitation and liquid-liquid extraction using 1,2-dichloroethane. Chromatographic separation of TIG and minocycline (internal standard, IS) was achieved on an Atlantis T3 column (150 mm × 3.0 mm, 3.0 μm) using gradient elution. The selected reaction monitoring transitions were performed at 293.60 m/z → 257.10 m/z for TIG and 458.00 m/z → 441.20 m/z for IS. The developed method was validated in terms of specificity, selectivity, linearity, lowest limit of quantification, limit of detection, precision, accuracy, matrix effect, carry-over effect, extraction recovery and stability. All parameters of the method submitted to validation met the acceptance criteria. The assay was linear over the concentration range of 0.01-100 μg/ml. This validated method was successfully applied to a TIG pharmacokinetic study in turkey after intravenous and oral administration at a dose of 10 mg/kg at various time-points.

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