Development of a specific fragment pattern-based quadrupole-Orbitrap mass spectrometry method to screen adulterated products of phosphodiesterase-5 inhibitors and their analogues

被引:16
作者
Lee, Ji Hyun [1 ]
Park, Han Na [1 ]
Park, Seongsoo [1 ]
Lee, Yong-Moon [2 ]
Kang, Hoil [1 ]
机构
[1] Minist Food & Drug Safety, Natl Inst Food & Drug Safety Evaluat, Div Adv Anal, Toxicol Evaluat & Res Dept, Cheongju 28159, Chungcheongbuk, South Korea
[2] Chungbuk Natl Univ, Coll Pharm, Cheongju 28159, Chungcheongbuk, South Korea
关键词
Q-Orbitrap-MS; Fragmentation pathways; PDE-5i analogue; Screening; Validation; Adulterated product; TADALAFIL ANALOG; DIETARY-SUPPLEMENTS; HEALTH SUPPLEMENTS; SILDENAFIL ANALOG; IDENTIFICATION; ELUCIDATION; VARDENAFIL; DRUGS; MS/MS;
D O I
10.1016/j.scijus.2019.02.006
中图分类号
DF [法律]; D9 [法律]; R [医药、卫生];
学科分类号
0301 ; 10 ;
摘要
Recently, adulterated supplements with phosphodiesterase-5 inhibitors (PDE-5i) have frequently observed. New synthetic analogues obtained from the chemical modification of parent compounds are frequently found in illicit products despite continuous efforts to inspect for these adulterants. A rapid and accurate method based on quadrupole-Orbitrap mass spectrometry was developed for simultaneously confirming and quantifying 85 PDE-5i and derived analogues present in illicit products for erectile dysfunction (ED). Common ions of PDE-5i according to their similar structures were proposed based on MS/MS fragmentations. These common ions could be an important diagnosis of their presence targets or new emerging analogues in supplements. Several validation parameters were employed, resulting in a limit of detection and quantification of 0.09-8.55 ng/mL and 0.24-17.10 ng/mL, respectively. The linear correlation coefficient (r(2)) was higher than 0.995, and mean recoveries of target compounds were in the range of 82-118%. A total of 187 illicit products, obtained from on/offline markets over a period of 3 years (2015-2017), were screened by the established method. Approximately 53% of them were adulterated with PDE-5i or derived analogues at concentrations of 0.1-726.0 mg/g in the illicit products. In the interests of public health, this study describes a rapid and accurate method to determine PDE-5i and new emerging analogues in adulterated products.
引用
收藏
页码:433 / 441
页数:9
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