Sreening of synthetic pharmaceutical drugs: PDE5 inhibitors, pain release, slimming groups in health supplements with LC-MS/MS

Linh Nguyen Trong, Nghia Cao Huu, Thi Chau Vinh
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Abstract

Nowadays, there were many reports from Viet nam & international laboratories have detected many kinds of undeclared synthesis drugs, even of banned-chemicals in health supplement products (HSP). We developed methods on LC-MS/MS to detect synthesis pharmaceutical drugs in following groups of HSP: strengthen sexual for man group: sildenafil, Tadalafil, Vardenafil; Anti- arthritis group: Dexamethasone, Prednisolon, Betamethasone, Piroxicam; Slimming group: Sibutramin, Orlistate, Phenophtalein, Furosemid. We carried out method validation of specificities & limit of dectections of above drugs on mass spectrometer system of Triple Quad SCiex 55000, analysis 80 samples of each group HSP were collected from 4 provinces: Dong nai, Binh Duong, Ba Ria- Vung Tau, Binh Phuoc in 2020. We validated fragment transition & LOD of each drugs: Sidenafil (mz 475.2 → 100.2/ 283.2), LOD: 0.015ppm;Tadanafil (mz 390.1 → 268.1/262.1) LOD: 0.015 ppm; Vadernafil (mz 483.9 → 312.3/299.2), LOD: 0.07ppm; Prednisolon (mz 361 → 147/343.3), LOD: 0.075ppm; Dexamethason (mz 393.2 → 373.1/293.1); LOD: 0.02 ppm; Betamethason (mz 393.1 → 147.1/355.2)LOD: 0.075 ppm; Piroxicam (mz 330 → 266.2/146.1); LOD: 0.015 ppm; Sibutramin (mz 280.9 → 139/125.2), LOD: 0.75 ppm; Orlistate (mz 496. → 179,2/ 114.1), LOD: 1 ppm; Phenophtalein (mz 319,2 → 141.1/283.2), LOD: 0.01 ppm; Furosemid (mz 329.2 → 285/204), LOD: 0.01 ppm. Screenning results: Sidenafil nondetected/80 samples; Tadalafil positive 10/80 samples, Vadernafil nondetected/80 samples in man sexual enhancement HSP; Prednisonlon nondetected /80 samples, Dexamethason nondetected /80 samples; Betamethason positive 1/80 samples, Piroxicam nondetected /80 samples in anti-arthritis HSP. Sibutramin & Phenolphtalein positive 7/80 samples, Orlistate nondetected/80 samples, Furosemid nondetected/80 samples in slimming HSP.
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用LC-MS/MS筛选保健品中合成药物:PDE5抑制剂、疼痛释放、减肥组
如今,有许多来自越南的报告,国际实验室在保健品(HSP)中发现了许多未申报的合成药物,甚至是禁用化学品。我们建立了LC-MS/MS检测以下组HSP合成药物的方法:男性组:西地那非、他达拉非、伐地那非;抗关节炎组:地塞米松、强的松、倍他米松、吡罗昔康;减肥组:西布曲明、奥利司他、酚他林、速尿。在sciex55000质谱系统上对上述药物的特异性和检出限进行了方法验证,分析了2020年在同奈、平阳、巴黎市-平头、平省4个省采集的每组HSP样品80份。我们验证了各药物的片段转换和LOD:西地那非(mz 475.2→100.2/ 283.2),LOD: 0.015ppm;他他那非(mz 390.1→268.1/262.1)LOD: 0.015ppm;vaderafil (mz 483.9→312.3/299.2),LOD: 0.07ppm;泼尼松龙(mz 361→147/343.3),LOD: 0.075ppm;地塞米松(mz 393.2→373.1/293.1);LOD: 0.02 ppm;倍他米松(mz 393.1→147.1/355.2)LOD: 0.075 ppm;吡洛昔康(mz330→266.2/146.1);LOD: 0.015 ppm;西布曲明(mz 280.9→139/125.2),LOD: 0.75 ppm;奥利司他(mz496)。→179,2/ 114.1),LOD: 1 ppm;Phenophtalein (mz 319,2→141.1/283.2),LOD: 0.01 ppm;Furosemid (mz 329.2→285/204),LOD: 0.01 ppm。筛选结果:Sidenafil未检出/80份;他达拉非阳性10/80例,伐地那非未检出80例;未检出泼尼松/80份,未检出地塞米松/80份;抗关节炎HSP中倍他米松阳性1/80,吡罗昔康未检出1/80。西布曲明和酚他林阳性7/80例,奥利司他未检出/80例,速尿未检出/80例。
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