title: Development and validation of UPLC and LC-MS/MS methods for the simultaneous determination of anti-obesity drugs in foods and dietary supplements.
abstract: Recently, the number of the cases in which weight loss products have been sold with illegal adulterants has increased, as awareness of the problems of obesity grows. In this study, we developed simultaneous analysis methods to rapidly and accurately identify ingredients illegally mixed with foods and dietary supplements. Twenty-three anti-obesity drugs in foods and dietary supplements were determined by developed and validated UPLC and LC-MS/MS methods. The UPLC method were validated for the LOD and LOQ in the ranges 0.05-3.0 and 0.2-10.0 μg/mL, respectively. The determination coefficient was over 0.999, precision was <6.2 %, and the accuracy was 80.8-103.9 %. The mean recoveries ranged from 80.3 to 109.3 % and RSD of stability was less than 2.1 %. The determination of the 23 anti-obesity drugs was accomplished by electrospray ionization LC-MS/MS using multiple reaction monitoring (MRM). The LODs and LOQs were in the ranges 0.03-7.5 and 0.09-30.0 ng/mL, respectively. The LC-MS/MS method was validated for linearity (r(2) > 0.99), precision (RSD < 10.7 %), accuracy (94.1-109.1 %), recovery (80.5-113.5 %), and the RSD of stability was <7.8 %. Using the newly developed and validated method, 193 samples were tested, and 55 were found to be adulterated.
authors.affiliation: Advanced Analysis Team, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety, 187, Osongeup, Heungdeok-gu, Cheongju-si, Chungcheongbuk-do, 363-700, Republic of Korea.
authors.forename: Jung Yeon
authors.initials: JY
authors.lastname: Kim
authors.affiliation: Advanced Analysis Team, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety, 187, Osongeup, Heungdeok-gu, Cheongju-si, Chungcheongbuk-do, 363-700, Republic of Korea.
authors.forename: Hyoung Joon
authors.initials: HJ
authors.lastname: Park
authors.affiliation: Advanced Analysis Team, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety, 187, Osongeup, Heungdeok-gu, Cheongju-si, Chungcheongbuk-do, 363-700, Republic of Korea.
authors.forename: Ji Won
authors.initials: JW
authors.lastname: Kim
authors.affiliation: Advanced Analysis Team, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety, 187, Osongeup, Heungdeok-gu, Cheongju-si, Chungcheongbuk-do, 363-700, Republic of Korea.
authors.forename: Ji Hyun
authors.initials: JH
authors.lastname: Lee
authors.affiliation: Advanced Analysis Team, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety, 187, Osongeup, Heungdeok-gu, Cheongju-si, Chungcheongbuk-do, 363-700, Republic of Korea.
authors.forename: Seok
authors.initials: S
authors.lastname: Heo
authors.affiliation: Advanced Analysis Team, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety, 187, Osongeup, Heungdeok-gu, Cheongju-si, Chungcheongbuk-do, 363-700, Republic of Korea.
authors.forename: Chang-Yong
authors.initials: CY
authors.lastname: Yoon
authors.affiliation: Advanced Analysis Team, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety, 187, Osongeup, Heungdeok-gu, Cheongju-si, Chungcheongbuk-do, 363-700, Republic of Korea. fly2thetop@hanmail.net.
authors.forename: Sooyeul
authors.initials: S
authors.lastname: Cho
mesh_terms: D019440:Anti-Obesity Agents / Q000032:analysis*; D002851:Chromatography, High Pressure Liquid / Q000379:methods / Q000592:standards / Q000639:trends; D002853:Chromatography, Liquid / Q000379:methods / Q000592:standards / Q000639:trends; D019587:Dietary Supplements / Q000032:analysis*; D005506:Food Contamination / Q000032:analysis*; D015203:Reproducibility of Results; D053719:Tandem Mass Spectrometry / Q000379:methods / Q000592:standards* / Q000639:trends*
chemical_list: D019440:Anti-Obesity Agents
keywords: Adulterant; Anti-obesity drug; LC-MS/MS; UPLC; Validated