CAJ | 학술논문

目的：建立超高效液相色谱-串联质谱法测定保健食品中西地那非、他达那非、伐地那非以及红地那非四种违禁药物含量的方法。方法采用ACQUITY UPLC BEH C18(100 mm×2.1 mm,1.7μm)色谱柱,以甲醇和添加0.1%甲酸5 mmol乙酸铵为流动相,梯度洗脱程序,进样分析20 min,在电喷雾正离子模式下以多反应监测(MRM)方式检测,外标法定量。结果四种那非类违禁药物的检出限(LOD, S/N=3)和定量限(LOD, S/N=10)分别0.1~0.5μg/kg 和0.3~2.0μg/kg 在0.1~100μg/kg 浓度范围内线性关系良好(r>0.99),加标回收率为73.6%~90.4%,相对标准偏差为1.0%~8.9%。结论该方法操作简单,重现性好,背景噪音低,具有较高的灵敏度和选择性。
목적：건립초고효액상색보-천련질보법측정보건식품중서지나비、타체나비、벌지나비이급홍지나비사충위금약물함량적방법。방법채용ACQUITY UPLC BEH C18(100 mm×2.1 mm,1.7μm)색보주,이갑순화첨가0.1%갑산5 mmol을산안위류동상,제도세탈정서,진양분석20 min,재전분무정리자모식하이다반응감측(MRM)방식검측,외표법정량。결과사충나비류위금약물적검출한(LOD, S/N=3)화정량한(LOD, S/N=10)분별0.1~0.5μg/kg 화0.3~2.0μg/kg 재0.1~100μg/kg 농도범위내선성관계량호(r>0.99),가표회수솔위73.6%~90.4%,상대표준편차위1.0%~8.9%。결론해방법조작간단,중현성호,배경조음저,구유교고적령민도화선택성。
Objective To develop a method for the simultaneous determination of sildenafil, tadalafil, vardenafil and acetildenafil in health-care foodstuffs by ultra performance liquid chromatography-mass spec-trometry. Methods The elution was separated on an ACQUITY UPLC BEH C18 column(100 mm×2.1 mm, 1.7μm) using the methanol-5 mmol ammonium acetate containing 0.1% formic acid as the mobile phase and a gradient elution program with a cycle time of 20 min, detected by electrospray ionization mass spectrometry in positive mode with multiple reaction monitoring, quantified by external standard method. Results The limits of detection(LOD, S/N=3)and quantification(LOQ, S/N=10) of 4 compounds were 0.1~0.5 μg/kg and 0.3~2.0μg/kg, respectively. The correlation coefficients of linear calibration curve were over 0.99 in the ranges of 0.1~100μg/kg. Average fortified recoveries were 73.6%~90.4%, and the relative standard deviations were in the ranges of 1.0%~8.9%. Conclusion This method has the advantages of simple operation, good reproduci-bility, low background noise, higher sensitivity and selectivity.