摘要
目的建立减肥类产品(含中成药、保健食品及食品)中N-丁基-3-(三氟甲基)-α-甲基苯乙胺的检测方法。方法采用超高效液相色谱串联线性离子阱质谱法,色谱柱为Waters ACQUITY UPLC®HSS T3柱(100 mm×2.1 mm,1.8μm),流动相为0.1%甲酸水溶液-0.1%甲酸-甲醇(梯度洗脱),流速为0.3 mL/min,检测波长为215 nm,柱温为30℃,进样量为1μL;电喷雾离子源、正电子模式(ESI+)。根据保留时间及离子对进行定性分析;利用多反应监测模式(MRM)拟合标准曲线,计算检出N-丁基-3-(三氟甲基)-α-甲基苯乙胺的含量。结果N-丁基-3-(三氟甲基)-α-甲基苯乙胺质量浓度在0.1~50 ng/mL范围内与定量离子对峰面积线性关系良好(r=1.0000);检测限为0.4 ng/g,定量限为1.2 ng/g;精密度、稳定性、重复性试验结果的RSD均小于3.0%;平均加样回收率为109.67%,RSD为5.46%(n=9)。结论该方法可特异、快速地检出减肥类产品中添加的N-丁基-3-(三氟甲基)-α-甲基苯乙胺,从而可应用于大批量样品的筛查与确证。
Objective To establish a method for the detection of N-{1-[3-(Trifluoromethyl)phenyl]-2-propanyl}-1-butanamine in the products for weight loss(including Chinese patent medicines,health food and food).Methods Ultra-high performance liquid chromatography tandem triple-quadrupole linear ion-trap mass spectrometry(UPLC-QTRAP-MS/MS)method was adopted.The chromatographic column was Waters ACQUITY UPLC®HSS T3 column(100 mm×2.1 mm,1.8μm),the mobile phase was 0.1%formic acid aqueous solution-0.1%formic acid-methanol(gradient elution),the flow rate was 0.3 mL/min,the detection wavelength was 215 nm,the column temperature was 30℃,and the injection volume was 1μL.The electro-spray ionization with positive mode(ESI+)was adopted.Qualitative analysis was conducted based on the retention time and ion pairs.The standard curve was fitted by the multiple reaction monitoring(MRM)mode,and the content of detected N-{1-[3-(Trifluoromethyl)phenyl]-2-propanyl}-1-butanamine was calculated.Results The linear range of N-{1-[3-(Trifluoromethyl)phenyl]-2-propanyl}-1-butanamine was 0.1-50 ng/mL(r=1.0000).The limit of detection was 0.4 ng/g,and the limit of quantification was 1.2 ng/g.The RSDs of precision,stability and repeatability tests were all lower than 3.0%.The average recovery rate of N-{1-[3-(Trifluoromethyl)phenyl]-2-propanyl}-1-butanamine was 109.67%,with an RSD of 5.46%(n=9).Conclusion The method can detect N-{1-[3-(Trifluoromethyl)phenyl]-2-propanyl}-1-butanamine specifically and rapidly in the products for weight loss,which can be used to the screening and confirmation of a large quantity of samples.
作者
方韵
贾昌平
张萍
张斌
FANG Yun;JIA Changping;ZHANG Ping;ZHANG Bin(Suzhou Institute for Drug Control,Suzhou,Jiangsu,China 215000;Wuhu Institute for Food and Drug Control,Wuhu,Anhui,China 241006)
出处
《中国药业》
CAS
2024年第4期85-89,共5页
China Pharmaceuticals
基金
安徽省药品监督管理局科技创新项目[AHYJ-KJ-202012]。
