Tags

Type your tag names separated by a space and hit enter

Development and implementation of a pass/fail field-friendly method for detecting sildenafil in suspect pharmaceutical tablets using a handheld Raman spectrometer and silver colloids.
J Pharm Biomed Anal. 2017 Nov 30; 146:420-425.JP

Abstract

A simple, fast, sensitive and effective pass/fail field-friendly method has been developed for detecting sildenafil in suspect Viagra and unapproved tablets using handheld Raman spectrometers and silver colloids. The method involves dissolving a portion of a tablet in water followed by filtration and addition of silver colloids, resulting in a solution that can be measured directly through a glass vial. Over one hundred counterfeit Viagra and unapproved tablets were examined on three different devices during the method development phase of the study. While the pass/fail approach was found to be 92.6% effective on average, the efficacy increased to 97.4% on average when coupled with the software's "Discover Mode" feature that allows the user to compare a suspect spectrum to that of a stored sildenafil spectrum. The lowest concentration of sildenafil in a water/colloid solution that yielded a "Pass" was found to be 7.6μg/mL or 7.6 parts per million (ppm). For the analysis of suspect tablets, this value was found to be as low as 10μg/mL and as high as 625μg/mL. This variability was likely related to the tablet formulation, e.g., concentration of sildenafil, presence and concentration of water-soluble and/or water-insoluble ingredients. However, since most counterfeit Viagra and unapproved tablets contain >50mg sildenafil per tablet, such low concentrations will not be encountered often. Limited in-lab and in-field validation studies were conducted in which analysts/field agents followed the procedure outlined in this study for small sample sets. These individuals were provided with written instructions, a ∼20min demonstration regarding how to perform the procedure and use the instrument, and a kit with field-friendly supplies (purified bottled water from a local grocery store, disposable plastic pipettes, eye-dropper with a silver colloid solution, etc.). The method proved to be 98.3% and 91.7% effective for the in-lab and in-field validation studies, respectively, which demonstrated the ruggedness, simplicity and practicality of the method.

Authors+Show Affiliations

U.S. Food and Drug Administration, Forensic Chemistry Center, Cincinnati, OH 45237, United States. Electronic address: adam.lanzarotta@yahoo.com.U.S. Food and Drug Administration, Forensic Chemistry Center, Cincinnati, OH 45237, United States.U.S. Food and Drug Administration, Forensic Chemistry Center, Cincinnati, OH 45237, United States.U.S. Food and Drug Administration, Forensic Chemistry Center, Cincinnati, OH 45237, United States.

Pub Type(s)

Journal Article

Language

eng

PubMed ID

28934694

Citation

Lanzarotta, Adam, et al. "Development and Implementation of a Pass/fail Field-friendly Method for Detecting Sildenafil in Suspect Pharmaceutical Tablets Using a Handheld Raman Spectrometer and Silver Colloids." Journal of Pharmaceutical and Biomedical Analysis, vol. 146, 2017, pp. 420-425.
Lanzarotta A, Lorenz L, Batson JS, et al. Development and implementation of a pass/fail field-friendly method for detecting sildenafil in suspect pharmaceutical tablets using a handheld Raman spectrometer and silver colloids. J Pharm Biomed Anal. 2017;146:420-425.
Lanzarotta, A., Lorenz, L., Batson, J. S., & Flurer, C. (2017). Development and implementation of a pass/fail field-friendly method for detecting sildenafil in suspect pharmaceutical tablets using a handheld Raman spectrometer and silver colloids. Journal of Pharmaceutical and Biomedical Analysis, 146, 420-425. https://doi.org/10.1016/j.jpba.2017.09.005
Lanzarotta A, et al. Development and Implementation of a Pass/fail Field-friendly Method for Detecting Sildenafil in Suspect Pharmaceutical Tablets Using a Handheld Raman Spectrometer and Silver Colloids. J Pharm Biomed Anal. 2017 Nov 30;146:420-425. PubMed PMID: 28934694.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Development and implementation of a pass/fail field-friendly method for detecting sildenafil in suspect pharmaceutical tablets using a handheld Raman spectrometer and silver colloids. AU - Lanzarotta,Adam, AU - Lorenz,Lisa, AU - Batson,JaCinta S, AU - Flurer,Cheryl, Y1 - 2017/09/08/ PY - 2017/07/05/received PY - 2017/09/01/revised PY - 2017/09/03/accepted PY - 2017/9/22/pubmed PY - 2018/5/31/medline PY - 2017/9/22/entrez KW - Counterfeit KW - Handheld Raman KW - Pass/Fail KW - SERS KW - Sildenafil KW - Surface enhanced Raman spectroscopy SP - 420 EP - 425 JF - Journal of pharmaceutical and biomedical analysis JO - J Pharm Biomed Anal VL - 146 N2 - A simple, fast, sensitive and effective pass/fail field-friendly method has been developed for detecting sildenafil in suspect Viagra and unapproved tablets using handheld Raman spectrometers and silver colloids. The method involves dissolving a portion of a tablet in water followed by filtration and addition of silver colloids, resulting in a solution that can be measured directly through a glass vial. Over one hundred counterfeit Viagra and unapproved tablets were examined on three different devices during the method development phase of the study. While the pass/fail approach was found to be 92.6% effective on average, the efficacy increased to 97.4% on average when coupled with the software's "Discover Mode" feature that allows the user to compare a suspect spectrum to that of a stored sildenafil spectrum. The lowest concentration of sildenafil in a water/colloid solution that yielded a "Pass" was found to be 7.6μg/mL or 7.6 parts per million (ppm). For the analysis of suspect tablets, this value was found to be as low as 10μg/mL and as high as 625μg/mL. This variability was likely related to the tablet formulation, e.g., concentration of sildenafil, presence and concentration of water-soluble and/or water-insoluble ingredients. However, since most counterfeit Viagra and unapproved tablets contain >50mg sildenafil per tablet, such low concentrations will not be encountered often. Limited in-lab and in-field validation studies were conducted in which analysts/field agents followed the procedure outlined in this study for small sample sets. These individuals were provided with written instructions, a ∼20min demonstration regarding how to perform the procedure and use the instrument, and a kit with field-friendly supplies (purified bottled water from a local grocery store, disposable plastic pipettes, eye-dropper with a silver colloid solution, etc.). The method proved to be 98.3% and 91.7% effective for the in-lab and in-field validation studies, respectively, which demonstrated the ruggedness, simplicity and practicality of the method. SN - 1873-264X UR - https://www.unboundmedicine.com/medline/citation/28934694/Development_and_implementation_of_a_pass/fail_field_friendly_method_for_detecting_sildenafil_in_suspect_pharmaceutical_tablets_using_a_handheld_Raman_spectrometer_and_silver_colloids_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0731-7085(17)31629-1 DB - PRIME DP - Unbound Medicine ER -