首页|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

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

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

UPLCQTRAP-MS/MSillegal additionN-{1-[3-(Trifluoromethyl)phenyl]-2-propanyl}-1-butanaminequalitative detectionquantitative detectionproduct for weight lossChinese patent medicinehealth foodfood

方韵、贾昌平、张萍、张斌

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江苏省苏州市药品检验检测研究中心,江苏 苏州 215000

安徽省芜湖市食品药品检验中心,安徽 芜湖 241006

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

安徽省药品监督管理局科技创新项目

AHYJ-KJ-202012

2024

10.3969/j.issn.1006-4931.2024.04.020

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
年,卷(期)：2024.33(4)
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