中国药业2024,Vol.33Issue(4) :85-89.DOI:10.3969/j.issn.1006-4931.2024.04.020

超高效液相色谱串联线性离子阱质谱法检测减肥类产品中N-丁基-3-(三氟甲基)-α-甲基苯乙胺

Detection of N-{1-[3-(Trifluoromethyl)Phenyl]-2-Propanyl}-1-Butanamine in Products for Weight Loss by UPLC-QTRAP-MS/MS

方韵 贾昌平 张萍 张斌
中国药业2024,Vol.33Issue(4) :85-89.DOI:10.3969/j.issn.1006-4931.2024.04.020

超高效液相色谱串联线性离子阱质谱法检测减肥类产品中N-丁基-3-(三氟甲基)-α-甲基苯乙胺

Detection of N-{1-[3-(Trifluoromethyl)Phenyl]-2-Propanyl}-1-Butanamine in Products for Weight Loss by UPLC-QTRAP-MS/MS

方韵 1贾昌平 1张萍 2张斌1
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作者信息

  • 1. 江苏省苏州市药品检验检测研究中心,江苏 苏州 215000
  • 2. 安徽省芜湖市食品药品检验中心,安徽 芜湖 241006
  • 折叠

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 = 1.000 0);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.

Abstract

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,1.8 µm),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 1 µL.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 = 1.000 0).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.

关键词

超高效液相色谱法/线性离子阱质谱法/非法添加/N-丁基-3-(三氟甲基)-α-甲基苯乙胺/定性检测/定量检测/减肥类产品/中成药/保健食品/食品

Key words

UPLC/QTRAP-MS/MS/illegal addition/N-{1-[3-(Trifluoromethyl)phenyl]-2-propanyl}-1-butanamine/qualitative detection/quantitative detection/product for weight loss/Chinese patent medicine/health food/food

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基金项目

安徽省药品监督管理局科技创新项目(AHYJ-KJ-202012)

出版年

2024
中国药业
重庆市食品药品监督管理局

中国药业

CSTPCD
影响因子:1.369
ISSN:1006-4931
参考文献量14
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