Simultaneous determination of illegal drug substances in dietary supplements for gout and osteoporosis using ultra-performance liquid chromatography and liquid chromatography-quadrupole-time-of-flight mass spectrometry.


Division of Advanced Analysis, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety, Osong Health Technology Administration Complex, 187 Osongsaengmyeong2-ro, Osongeup, Heungdeok-gu, Cheongju-si, Chungcheongbuk-do, 363-700, Republic of Korea. Electronic address: [Email]


The aim of this study was to simultaneously determine the presence of unauthorized drug substances in health foods and herbal products used in the treatment of conditions such as gout and anti-osteoporosis. Therefore, we developed and optimised a rapid and accurate method to simultaneously measure 20 anti-gout and anti-osteoporosis drug substances using an ultra-high-performance liquid chromatography (UPLC) system equipped with a photodiode array (PDA) detector. The method was validated to fully meet internationally accepted standards. LODs and LOQs spiked in solid and liquid negative samples were ranged from 0.12 to 1.50 μg/mL, and ranged from 0.36 to 4.50 μg/mL. Linearities (R2> 0.999), stabilities (RSD ≤ 2.92%), accuracies (84.25∼106.62%, intra-day; 84.56∼105.85%, inter-day), precisions (RSD ≤ 3.71% on the intra-day; RSD ≤ 3.47% on the inter-day), recoveries spiked in various type of blank samples such as powder, liquid, tablet, and capsule were determined within 81.20-116.20 %, respectively. From a confirmation of matrix effects (88.06∼110.50% in solid blank; 89.16∼110.52% in liquid blank), it was confirmed that this method was not significantly affected by a sample matrix. The validated method was used to analyse 116 samples containing health foods, herbal products, and seized forensic samples advertised to be effective anti-gout and anti-osteoporosis agents. Of the 20 drug substances screened, dexamethasone was detected and confirmed by comparing the tandem mass spectrometry (MS/MS) fragment ion patterns of a reference standard and the sample using LC-quadrupole-time-of-flight (Q-TOF)/MS. The concentrations of adulterants in seized forensic samples ranged from 0.013 to 0.022 %.



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