CAJ | 학술논문

改造有明确疗效的药物，合成新的衍生物以避开法定检验方法是目前化学药物非法添加的趋势之一。本文提出将液相色谱-三重四极杆质谱联用仪的质谱前体离子扫描模式应用于中药及保健食品等复杂体系中非法添加药物衍生物的快速筛查策略，以5型磷酸二酯酶抑制剂为实验对象，通过分析该类化合物的结构和质谱特点将其分类，筛选各类共有的子离子碎片，优化质谱参数，建立了前体离子扫描模式的 LC-MS 筛查方法，讨论了质谱参数和碎片离子的选择对筛选结果的影响，并应用于实际样品的测定。结果表明，该方法既可以满足已知化合物的测定需要，又可以对复杂体系中未知的同类衍生物进行快速筛查，防止未知衍生物的漏检。该方法灵敏、专属、高效，值得进一步研究。
개조유명학료효적약물，합성신적연생물이피개법정검험방법시목전화학약물비법첨가적추세지일。본문제출장액상색보-삼중사겁간질보련용의적질보전체리자소묘모식응용우중약급보건식품등복잡체계중비법첨가약물연생물적쾌속사사책략，이5형린산이지매억제제위실험대상，통과분석해류화합물적결구화질보특점장기분류，사선각류공유적자리자쇄편，우화질보삼수，건립료전체리자소묘모식적 LC-MS 사사방법，토론료질보삼수화쇄편리자적선택대사선결과적영향，병응용우실제양품적측정。결과표명，해방법기가이만족이지화합물적측정수요，우가이대복잡체계중미지적동류연생물진행쾌속사사，방지미지연생물적루검。해방법령민、전속、고효，치득진일보연구。
The compounds with similar structure often have similar pharmacological activities. So it is a trend for illegal addition that new derivatives of effective drugs are synthesized to avoid the statutory test. This bring challenges to crack down on illegal addition behavior, however,modified derivatives usually have similar product ions,which allow for precursor ion scanning. In this work,precursor ion scanning mode of a triple quadrupole mass spectrometer was first applied to screen illegally added drugs in complex matrix such as Chinese traditional patent medicines and healthy foods. Phosphodiesterase-5 inhibitors were used as experimental examples. Through the analysis of the structure and mass spectrum characteristics of the com-pounds,phosphodiesterase-5 inhibitors were classified,and their common product ions were screened by full scan of product ions of typical compounds. Then high performance liquid chro-matography-tandem mass spectrometry( HPLC-MS / MS)method with precursor ion scanning mode was established based on the optimization of MS parameters. The effect of mass parame-ters and the choice of fragment ions were also studied. The method was applied to determine actual samples and further refined. The results demonstrated that this method can meet the need of rapid screening of unknown derivatives of phosphodiesterase-5 inhibitors in complex matrix,and prevent unknown derivatives undetected. This method shows advantages in sensi-tivity,specificity and efficiency,and is worth to be further investigated.