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REFERENCES
Gloria S. Chung, Dr. Lyman Rickard
Department of Chemistry, Millersville University, Millersville, PA 17551
This study consists of troubleshooting, calibrating, and optimizing a liquid
chromatography/mass spectrometer (LC/MS), a new addition to the Chemistry
Department’s analytical capabilities. LC/MS is an analytical separation technique that
is widely used in industry. This instrument is highly sensitive and is capable of accurate
quantitative determinations. Other benefits include the capability of separating
nonvolatile species. A major part of this project will be the development and
optimization of the separation and quantification of parabens in personal care products.
This procedure will be utilized in an upper level Analytical Chemistry lab course.
Dr. Lyman H. Rickard
Dr. Daniel R. Albert
Mr. Stephen W. Peurifoy
President Dr. John Anderson
Tom Blackwell
U.S. Drug Enforcement Agency (Northeast Testing Lab, New York, NY)
EXPERIMENTAL PROCEDURE
Separation of Paraben Preservatives by Reversed-Phase HPLC; Coral Barbas, Javier Ruperez, Andre Dams, and Ronal E.
Majors; Agilent Technologies. Applications Note.
“Development and Validation of a Fast Procedure To Analyze Amoxicillin in River Waters by Direct-Injection LC-MS/MS”,
V Homem, AAlves, and L Santos, J. Chem. Ed., 2014, 91, 1961-1965.
“Development of A Validated HPLC Method for the Analysis of Two Preservative Agents ‘Methylparaben & Propylparaben’
in Topical Creams Containing Steroids in the Patient’s Terms of Use”, B. Arous and M. A. Al-Mardini, Int. J. Pharm.
Sci. Rev. Res., 22(2), Sep – Oct 2013; n 36, 200-205.
Rubinson, Kenneth A. and Rubinson, Judith F. Contemporary Instrumental Analysis. Upper Saddle River, NJ: Prentice Hall,
2000. Print.
BACKGROUND
The purpose of the experimental method is to separate and quantify parabens in personal care
products using LC/MS. The sample chosen for analysis was Crest Pro Health CPC
Antigingivitis/Antiplaque Oral Rinse. The procedure measures the concentrations of methyl
paraben and propyl paraben by standard addition. The reagents used in this experiment include
the following: methyl paraben and propyl paraben standard solutions, acetonitrile, and methanol.
Samples are prepared by pipeting a constant volume of dissolved personal care product into a
series of volumetric flasks followed by the addition of varying volumes of standard methyl
paraben and propyl paraben. All volumetric flasks are then diluted to the calibration mark with
solvent. Sample solutions are then injected into the LC/MS where they are separated into their
components and each component analyzed by the mass spectrometer.
High Performance Liquid Chromatography (HPLC) is a widely used analytical
separation technique due to its sensitivity, adaptability to accurate quantitative
determinations, ease of automation, suitability for separating nonvolatile species, and its
wide applicability to substances that are important to industry. The technique used to
measure the masses of ions and their abundances in the gas phase is known as mass
spectrometry (MS). Liquid chromatography/mass spectrometry is the combination of
these two analytical techniques. The HPLC separates mixtures into their components
and the mass spectrometer is used for qualitative and quantitative analysis of each
component.
Liquid Chromatography (LC) is a technique to separate a sample into its individual
components. The separation of LC consists of mobile and stationary phases. The mobile
phase carries the sample into a column, where the sample then partitions. This allows
the separation into the sample’s components. The polarities of the compounds are
determined based on the polarities of the stationary and mobile phases.
Mass spectrometry is a versatile and powerful tool for chemical analysis. The operation
sequence of the MS involves generation of gas-phase molecules, ionization of the
molecules followed by fragmentation, separation of ions based on mass-to-charge ratio,
and detection of the ion beam. Figure 1 displays the major components of a mass
spectrometer. Components of the sample mixture exit the chromatographic column and
enter the source of the mass spectrometer where the molecules vaporized and ionized.
The ions are accelerated across an electric field. The accelerated ions then pass from the
source to the quadrupole mass analyzer, where the ions of different masses are
separated.
Determining the Concentration of Parabens in Personal Care
Products Using the LC/MS
ABSTRACT
Figure 1: Three major
components of a mass
spectrometer.
BACKGROUND (cont.)
Parabens, shown in Figure 2, are preservatives, which are used in many personal care products
to increase shelf life. Besides increasing shelf life, parabens prevent contamination and bacterial
growth during use, thus, reducing undesirable chemical changes and product damage from
microorganisms. Furthermore, parabens prevent degradation, irritation, and infection. Parabens
are added at low levels for safety reasons. There are safety concerns associated with the use of
parabens, even though they have antimicrobial activities and low toxicity. Parabens can have
adverse health effects, such as a potential cause of breast cancer and reduction of sperm count
and testosterone levels. According to the United States Food and Drug Administration (FDA),
many personal care products contain low levels of parabens but that they cause no harm at these
low concentrations. Because of these potential health risks, the determination of parabens as
well as other preservatives in personal care products is important.
Figure 2: Chemical structure of parabens with
different R-groups. The general structure is an alkyl
esters of p-hydroxybenzoic acid.
BLOCK DIAGRAM OF INSTRUMENTATION
Mass
Analyzer Detector
Data Analysis
Mobile Phase
Pump Injector Column
ACKNOWLEDGEMENTS

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Made in Millersville: Determining the Concentration of Parabens in Personal Care Products Using the LC/MS

  • 1. REFERENCES Gloria S. Chung, Dr. Lyman Rickard Department of Chemistry, Millersville University, Millersville, PA 17551 This study consists of troubleshooting, calibrating, and optimizing a liquid chromatography/mass spectrometer (LC/MS), a new addition to the Chemistry Department’s analytical capabilities. LC/MS is an analytical separation technique that is widely used in industry. This instrument is highly sensitive and is capable of accurate quantitative determinations. Other benefits include the capability of separating nonvolatile species. A major part of this project will be the development and optimization of the separation and quantification of parabens in personal care products. This procedure will be utilized in an upper level Analytical Chemistry lab course. Dr. Lyman H. Rickard Dr. Daniel R. Albert Mr. Stephen W. Peurifoy President Dr. John Anderson Tom Blackwell U.S. Drug Enforcement Agency (Northeast Testing Lab, New York, NY) EXPERIMENTAL PROCEDURE Separation of Paraben Preservatives by Reversed-Phase HPLC; Coral Barbas, Javier Ruperez, Andre Dams, and Ronal E. Majors; Agilent Technologies. Applications Note. “Development and Validation of a Fast Procedure To Analyze Amoxicillin in River Waters by Direct-Injection LC-MS/MS”, V Homem, AAlves, and L Santos, J. Chem. Ed., 2014, 91, 1961-1965. “Development of A Validated HPLC Method for the Analysis of Two Preservative Agents ‘Methylparaben & Propylparaben’ in Topical Creams Containing Steroids in the Patient’s Terms of Use”, B. Arous and M. A. Al-Mardini, Int. J. Pharm. Sci. Rev. Res., 22(2), Sep – Oct 2013; n 36, 200-205. Rubinson, Kenneth A. and Rubinson, Judith F. Contemporary Instrumental Analysis. Upper Saddle River, NJ: Prentice Hall, 2000. Print. BACKGROUND The purpose of the experimental method is to separate and quantify parabens in personal care products using LC/MS. The sample chosen for analysis was Crest Pro Health CPC Antigingivitis/Antiplaque Oral Rinse. The procedure measures the concentrations of methyl paraben and propyl paraben by standard addition. The reagents used in this experiment include the following: methyl paraben and propyl paraben standard solutions, acetonitrile, and methanol. Samples are prepared by pipeting a constant volume of dissolved personal care product into a series of volumetric flasks followed by the addition of varying volumes of standard methyl paraben and propyl paraben. All volumetric flasks are then diluted to the calibration mark with solvent. Sample solutions are then injected into the LC/MS where they are separated into their components and each component analyzed by the mass spectrometer. High Performance Liquid Chromatography (HPLC) is a widely used analytical separation technique due to its sensitivity, adaptability to accurate quantitative determinations, ease of automation, suitability for separating nonvolatile species, and its wide applicability to substances that are important to industry. The technique used to measure the masses of ions and their abundances in the gas phase is known as mass spectrometry (MS). Liquid chromatography/mass spectrometry is the combination of these two analytical techniques. The HPLC separates mixtures into their components and the mass spectrometer is used for qualitative and quantitative analysis of each component. Liquid Chromatography (LC) is a technique to separate a sample into its individual components. The separation of LC consists of mobile and stationary phases. The mobile phase carries the sample into a column, where the sample then partitions. This allows the separation into the sample’s components. The polarities of the compounds are determined based on the polarities of the stationary and mobile phases. Mass spectrometry is a versatile and powerful tool for chemical analysis. The operation sequence of the MS involves generation of gas-phase molecules, ionization of the molecules followed by fragmentation, separation of ions based on mass-to-charge ratio, and detection of the ion beam. Figure 1 displays the major components of a mass spectrometer. Components of the sample mixture exit the chromatographic column and enter the source of the mass spectrometer where the molecules vaporized and ionized. The ions are accelerated across an electric field. The accelerated ions then pass from the source to the quadrupole mass analyzer, where the ions of different masses are separated. Determining the Concentration of Parabens in Personal Care Products Using the LC/MS ABSTRACT Figure 1: Three major components of a mass spectrometer. BACKGROUND (cont.) Parabens, shown in Figure 2, are preservatives, which are used in many personal care products to increase shelf life. Besides increasing shelf life, parabens prevent contamination and bacterial growth during use, thus, reducing undesirable chemical changes and product damage from microorganisms. Furthermore, parabens prevent degradation, irritation, and infection. Parabens are added at low levels for safety reasons. There are safety concerns associated with the use of parabens, even though they have antimicrobial activities and low toxicity. Parabens can have adverse health effects, such as a potential cause of breast cancer and reduction of sperm count and testosterone levels. According to the United States Food and Drug Administration (FDA), many personal care products contain low levels of parabens but that they cause no harm at these low concentrations. Because of these potential health risks, the determination of parabens as well as other preservatives in personal care products is important. Figure 2: Chemical structure of parabens with different R-groups. The general structure is an alkyl esters of p-hydroxybenzoic acid. BLOCK DIAGRAM OF INSTRUMENTATION Mass Analyzer Detector Data Analysis Mobile Phase Pump Injector Column ACKNOWLEDGEMENTS