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Marcello Chiarotti - One of the best experts on this subject based on the ideXlab platform.
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Ultra high performance liquid chromatography–electrospray ionization–tandem mass spectrometry screening method for direct analysis of designer drugs, “spice” and stimulants in oral fluid
Journal of Chromatography A, 2012Co-Authors: Sabina Strano-rossi, Luca Anzillotti, Erika Castrignanò, Francesco Saverio Romolo, Marcello ChiarottiAbstract:An ultra high performance liquid chromatography–electrospray ionization–tandem mass spectrometry (UHPLC–ESI–MS/MS) screening method for the direct analysis in oral fluid (OF) of 24 drugs, including new synthetic cannabinoids and so-called “smart” designer drugs, in a single chromatographic run was set up. Benzylpiperazine, methylone, 5,6-methylenedioxy-2-aminoindane (MDAI), Fenproporex, 4-fluoroamphetamine (4-FA), 4-methyl-N-ethylcathinone (4-MEC), 4-methylamphetamine (4-MA), methylbenzodioxolylbutanamine (MBDB), mephedrone, methylthioamphetamine (MTA), methylenedioxypyrovalerone (MDPV), mefenorex, nabilone, furfenorex, clobenzorex, JWH-200, AM 694, JWH-250, JWH-073, JWH-018, JWH-019, JWH-122, HU 210 and CP 47497 were determined in a chromatographic run of 9 min only with no sample pre-treatment, after addition of ISs and dilution in mobile phase A. This method is designed to be applied to 250 μL of OF sample, anyway is suitable to be used on smaller volumes (till 100 μL). LODs vary from 1 ng/mL to 20 ng/mL. No interfering peaks were observed due to similar analytes, common therapeutic drugs or endogenous compounds. Matrix effect, although present especially for mephedrone, is acceptable, allowing the detection of the compounds at the LODs described. The developed method was applied on 400 real OF samples from on-site tests performed by police officers.
Pedro Eduardo Froehlich - One of the best experts on this subject based on the ideXlab platform.
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validation and application of a liquid chromatography electrospray ionization mass spectrometric method for determination of mazindol in human plasma and urine
Journal of Pharmacological and Toxicological Methods, 2016Co-Authors: Marcella Herbstrith De Oliveira, Pâmela Lukasewicz C Ferreira, Graciela Carlos, Fernanda Rodrigues Salazar, Ana Maria Bergold, Renata Pereira Limberger, Flavio Pechansky, Pedro Eduardo FroehlichAbstract:Abstract Introduction Even after removal of some stimulants, like Fenproporex, amfepramone and mazindol, from Brazilian market, the use of these substances is still high, especially by drivers. Mazindol is the second most used anorectic agent in the world acting as an indirect sympathomimetic agonist, having stimulatory action on central nervous system. Plasma is a good matrix to monitor since it reflects the psychomotor effects of these drugs, but unlike urine has an invasive collection; drug levels and detection time are quite low. Method The method involved a liquid–liquid extraction of the samples and a LC–MS analysis was fully validated. Method was used to analyze samples of urine and plasma collected from health volunteers in a period of 24 h. Metabolite of mazindol was synthesized using alkaline conditions. Results After validation the method proved to be adequate to analyze samples collected from health volunteers. Method was linear in the concentration range of 0.1–10 ng/mL (r = 0.9982) for plasma and 5–50 ng/mL (r = 0.9973) for urine. Discussion Analysis of the samples showed that mazindol can be detected after 1 h of administration and that concentration levels in urine were always higher than in plasma. Mazindol metabolite was detected only in urine.
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determination of mazindol in human oral fluid by high performance liquid chromatography electrospray ionization mass spectrometry
Biomedical Chromatography, 2014Co-Authors: Marcella Herbstrith De Oliveira, Graciela Carlos, Ana Maria Bergold, Renata Pereira Limberger, Flavio Pechansky, Pedro Eduardo FroehlichAbstract:Brazil is one of the countries most affected by abuse of stimulant medications by professional drivers, especially Fenproporex, amfepramone and mazindol. Even though their sale is banned, they can be found in illegal markets, such as those located on the country's borders. The use of oral fluid to monitor drug levels has many advantages over plasma and urine because it is noninvasive, easier to collect and more difficult to adulterate. The aim of this study was to develop and validate a sensitive and specific method to quantify mazindol in human oral fluid by liquid chromatography-mass spectrometry (LC-MS). The LC system consisted of an LC-MS system operated in selected ion monitoring mode. The mobile phase was composed of water at pH 4.0, acetonitrile and methanol (60:15:25 v/v/v) at a flow rate of 1.0 mL/min and propranolol was used as internal standard. Total running time was 10 min. The lower limit of quantification was 0.2 ng/mL and the method exhibited good linearity within the 0.2-20 ng/mL range (r = 0.9987). A rapid, specific, sensitive, linear, precise and accurate method was developed for determination of mazindol in human oral fluid according to European Medicines Agency guidelines, and is suitable for monitoring mazindol levels in oral fluid of professional drivers. Language: en
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Development and Validation of an LC-UV Method for Quantitation of 4-Bromo-2,5-Dimethoxyamphetamine (DOB), 4-Bromo-2,5-Dimethoxyphenetylamine (2C-B), Methylphenidate, Fenproporex and Amfepramone
Chromatographia, 2009Co-Authors: Maria Cristina Franck, Renata Pereira Limberger, Leonardo Zanchetti Meneghini, Luciana Rossato, Pedro Eduardo FroehlichAbstract:A sensitive and reliable isocratic LC-UV method was developed and validated for quantification of 4-bromo-2,5-dimethoxyamphetamine (DOB), 4-bromo-2,5-dimethoxyphenetylamine (2C-B), amfepramone (diethylpropione, DEP), Fenproporex (FEN) and methylphenidate (MPH). Although these substances are not usually associated, the fact that the same method could be used to analyze five different amphetamines would be very helpful in forensic analysis. The validation parameters accessed were linearity, specificity, precision, accuracy, limit of detection, limit of quantification and robustness. During the evaluation of selectivity, benzaldehyde (BZ) and N-methyl-diethanolamine (MDEA), two out of nine related substances tested, did not show good resolution from DOB and FEN, respectively. However, commercial preparations containing DEP, FEN and MPH were analyzed and no interference from their excipients was noticed. Through this method, these five amphetamine derivatives studied were simultaneously identified and quantified. The developed method is easy to implement, fast and suitable for use in routine laboratory analysis. The only limitation would be the quantitation of DOB and FEN in the presence of large amounts of BZ and MDEA, respectively.
Sabina Strano-rossi - One of the best experts on this subject based on the ideXlab platform.
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Ultra high performance liquid chromatography–electrospray ionization–tandem mass spectrometry screening method for direct analysis of designer drugs, “spice” and stimulants in oral fluid
Journal of Chromatography A, 2012Co-Authors: Sabina Strano-rossi, Luca Anzillotti, Erika Castrignanò, Francesco Saverio Romolo, Marcello ChiarottiAbstract:An ultra high performance liquid chromatography–electrospray ionization–tandem mass spectrometry (UHPLC–ESI–MS/MS) screening method for the direct analysis in oral fluid (OF) of 24 drugs, including new synthetic cannabinoids and so-called “smart” designer drugs, in a single chromatographic run was set up. Benzylpiperazine, methylone, 5,6-methylenedioxy-2-aminoindane (MDAI), Fenproporex, 4-fluoroamphetamine (4-FA), 4-methyl-N-ethylcathinone (4-MEC), 4-methylamphetamine (4-MA), methylbenzodioxolylbutanamine (MBDB), mephedrone, methylthioamphetamine (MTA), methylenedioxypyrovalerone (MDPV), mefenorex, nabilone, furfenorex, clobenzorex, JWH-200, AM 694, JWH-250, JWH-073, JWH-018, JWH-019, JWH-122, HU 210 and CP 47497 were determined in a chromatographic run of 9 min only with no sample pre-treatment, after addition of ISs and dilution in mobile phase A. This method is designed to be applied to 250 μL of OF sample, anyway is suitable to be used on smaller volumes (till 100 μL). LODs vary from 1 ng/mL to 20 ng/mL. No interfering peaks were observed due to similar analytes, common therapeutic drugs or endogenous compounds. Matrix effect, although present especially for mephedrone, is acceptable, allowing the detection of the compounds at the LODs described. The developed method was applied on 400 real OF samples from on-site tests performed by police officers.
Francesco Saverio Romolo - One of the best experts on this subject based on the ideXlab platform.
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Ultra high performance liquid chromatography–electrospray ionization–tandem mass spectrometry screening method for direct analysis of designer drugs, “spice” and stimulants in oral fluid
Journal of Chromatography A, 2012Co-Authors: Sabina Strano-rossi, Luca Anzillotti, Erika Castrignanò, Francesco Saverio Romolo, Marcello ChiarottiAbstract:An ultra high performance liquid chromatography–electrospray ionization–tandem mass spectrometry (UHPLC–ESI–MS/MS) screening method for the direct analysis in oral fluid (OF) of 24 drugs, including new synthetic cannabinoids and so-called “smart” designer drugs, in a single chromatographic run was set up. Benzylpiperazine, methylone, 5,6-methylenedioxy-2-aminoindane (MDAI), Fenproporex, 4-fluoroamphetamine (4-FA), 4-methyl-N-ethylcathinone (4-MEC), 4-methylamphetamine (4-MA), methylbenzodioxolylbutanamine (MBDB), mephedrone, methylthioamphetamine (MTA), methylenedioxypyrovalerone (MDPV), mefenorex, nabilone, furfenorex, clobenzorex, JWH-200, AM 694, JWH-250, JWH-073, JWH-018, JWH-019, JWH-122, HU 210 and CP 47497 were determined in a chromatographic run of 9 min only with no sample pre-treatment, after addition of ISs and dilution in mobile phase A. This method is designed to be applied to 250 μL of OF sample, anyway is suitable to be used on smaller volumes (till 100 μL). LODs vary from 1 ng/mL to 20 ng/mL. No interfering peaks were observed due to similar analytes, common therapeutic drugs or endogenous compounds. Matrix effect, although present especially for mephedrone, is acceptable, allowing the detection of the compounds at the LODs described. The developed method was applied on 400 real OF samples from on-site tests performed by police officers.
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Ultra high performance liquid chromatography–electrospray ionization–tandem mass spectrometry screening method for direct analysis of designer drugs, “spice” and stimulants in oral fluid
'Elsevier BV', 2012Co-Authors: Strano Rossi Sabina, Francesco Saverio Romolo, Anzillotti L, Chiarotti MarcelloAbstract:An ultra high performance liquid chromatography\u2013electrospray ionization\u2013tandem mass spectrometry (UHPLC\u2013ESI\u2013MS/MS) screening method for the direct analysis in oral fluid (OF) of 24 drugs, including new synthetic cannabinoids and so-called \u201csmart\u201d designer drugs, in a single chromatographic run was set up. Benzylpiperazine, methylone, 5,6-methylenedioxy-2-aminoindane (MDAI), Fenproporex, 4-fluoroamphetamine (4-FA), 4-methyl-N-ethylcathinone (4-MEC), 4-methylamphetamine (4-MA), methylbenzodioxolylbutanamine (MBDB), mephedrone, methylthioamphetamine (MTA), methylenedioxypyrovalerone (MDPV), mefenorex, nabilone, furfenorex, clobenzorex, JWH-200, AM 694, JWH-250, JWH-073, JWH-018, JWH-019, JWH-122, HU 210 and CP 47497 were determined in a chromatographic run of 9 min only with no sample pre-treatment, after addition of ISs and dilution in mobile phase A. This method is designed to be applied to 250 L of OF sample, anyway is suitable to be used on smaller volumes (till 100 L). LODs vary from 1 ng/mL to 20 ng/mL. No interfering peaks were observed due to similar analytes, common therapeutic drugs or endogenous compounds. Matrix effect, although present especially for mephedrone, is acceptable, allowing the detection of the compounds at the LODs described. The developed method was applied on 400 real OF samples from on-site tests performed by police officers
Erika Castrignanò - One of the best experts on this subject based on the ideXlab platform.
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Ultra high performance liquid chromatography–electrospray ionization–tandem mass spectrometry screening method for direct analysis of designer drugs, “spice” and stimulants in oral fluid
Journal of Chromatography A, 2012Co-Authors: Sabina Strano-rossi, Luca Anzillotti, Erika Castrignanò, Francesco Saverio Romolo, Marcello ChiarottiAbstract:An ultra high performance liquid chromatography–electrospray ionization–tandem mass spectrometry (UHPLC–ESI–MS/MS) screening method for the direct analysis in oral fluid (OF) of 24 drugs, including new synthetic cannabinoids and so-called “smart” designer drugs, in a single chromatographic run was set up. Benzylpiperazine, methylone, 5,6-methylenedioxy-2-aminoindane (MDAI), Fenproporex, 4-fluoroamphetamine (4-FA), 4-methyl-N-ethylcathinone (4-MEC), 4-methylamphetamine (4-MA), methylbenzodioxolylbutanamine (MBDB), mephedrone, methylthioamphetamine (MTA), methylenedioxypyrovalerone (MDPV), mefenorex, nabilone, furfenorex, clobenzorex, JWH-200, AM 694, JWH-250, JWH-073, JWH-018, JWH-019, JWH-122, HU 210 and CP 47497 were determined in a chromatographic run of 9 min only with no sample pre-treatment, after addition of ISs and dilution in mobile phase A. This method is designed to be applied to 250 μL of OF sample, anyway is suitable to be used on smaller volumes (till 100 μL). LODs vary from 1 ng/mL to 20 ng/mL. No interfering peaks were observed due to similar analytes, common therapeutic drugs or endogenous compounds. Matrix effect, although present especially for mephedrone, is acceptable, allowing the detection of the compounds at the LODs described. The developed method was applied on 400 real OF samples from on-site tests performed by police officers.