减肥类中成药、保健食品、食品中非法添加酚酞、西布曲明等化学成分的快筛检测方法研究

目的 建立快筛检测减肥类中成药、保健食品和食品中非法添加酚酞、西布曲明等化学成分的方法.方法 用快筛试管法和薄层色谱法检测产品所含的酚酞、西布曲明等化学成分,并通过HPLC-DAD/HPLC-MS确认.结果 103批次产品中42批次检出酚酞,61批次检出西布曲明,其他相关化学成分目前均未检出.结论 此方法专属性强、灵敏度高、重现性好,是一种简便快捷、经济实用、准确判断减肥类产品是否非法添加酚酞、西布曲明等化学成分的快筛检测方法,适用于快速鉴别筛查基层大批量产品.     

减肥保健食品中非法添加酚酞和西布曲明的同时检测

目的：建立测定减肥保健食品中非法添加酚酞和西布曲明的高效液相色谱- 串联质谱分析方法,并通过研究其质谱特征,推测其裂解途径。方法：减肥咖啡、减肥茶、减肥胶囊、苹果醋咀嚼片、减肥蛋白素等不同类型的减肥保健食品经超声波辅助提取15min,以Waters Atlantis T3 柱(150mm × 2.1mm,3μm)分离后,进行HPLCMS/MS 多反应监测模式下的定性及定量分析。结果：酚酞在2.5～500μg/L 的范围内呈良好的线性关系,相关系数为0.9992;西布曲明在0.15～500μg/L 的范围内呈良好的线性关系,相关系数为0.9996。在低、中、高3 个添加水平范围内的平均回收率为82.3%～103.6%;日内精密度均小于5%,日间精密度均小于8%。在检测的20 种样品中,检出含有西布曲明的样品13 个,检出率为65%;含有酚酞的样品9 个,检出率为45%。结论：本方法分析速度快、灵敏度高、回收率好,可用于不同减肥保健食品中非法添加酚酞和西布曲明的同时检测。     

减肥保健食品中非法添加盐酸西布曲明的检测

建立减肥保健食品中非法添加化学成分盐酸西布曲明的定性、定量检测方法.采用薄层色谱法、高幸合嗌?二极管阵列检测法、LC/MS/MS联用技术进行定性鉴别,并采用高效液相色谱法测定其中盐酸西布曲明的含量.结果在抽取的43种市售产品中,有9种检出了盐酸西布曲明.该方法快速、简便、准确、可靠,可用于有效监测保健食品中非法添加的盐酸西布曲明.     

拉曼光谱快速检测减肥保健品中非法添加酚酞的研究

目的:采用拉曼光谱法快速检测减肥保健品中非法添加的酚酞。方法:采用拉曼光谱对减肥保健品中的非法添加物质酚酞进行快速检测,首先使用适当的溶剂对减肥保健品进行提取,然后对提取液进行过滤,最后直接进行拉曼光谱的测试。结果:建立了酚酞-甲醇溶液的标准曲线,并且对添加不同浓度酚酞的减肥保健品进行拉曼光谱检测,所得结果与酚酞实际添加量一致。结论:结合简单的前处理方法,拉曼光谱法可对减肥保健品中非法添加的酚酞进行快速检测,并可进行定量分析;该方法快速、简便、成本低、可同时得到定性与定量结果,该方法的检测限为1%。     

解吸附电晕束电离质谱辅助高效液相色谱法检测减肥类保健食品中的违禁药物

目的利用解吸附电晕束电离质谱(DCBI-MS)对减肥类保健食品中违禁药物进行快速筛选,进而用高效液相色谱法(HPLC-UV)对疑似检出样品准确定量。方法通过DCBI-MS直接分析,对比标准物质的一级、二级质谱谱图,对检测样品中非法添加的芬氟拉明、酚酞、西布曲明、单去甲基西布曲明、双去甲基西布曲明进行定性鉴别。HPLC-UV对5种目标化合物准确定量。结果 HPLC-UV方法中各目标物的线性范围为0.25～300 mg/L。12个检测样品中3个样品共3种违禁物被DCBI-MS方法检出。高效液相色谱法准确复检结果显示DCBI-MS的半定量结果可信。结论 DCBI-MS无需样品预处理,单个样品的分析时间不到1 min,辅助高效液相色谱法实现了减肥类违禁药物的快速、高通量、高精度检测。     

电喷雾-离子迁移谱快速检测减肥类保健食品中非法添加的22种化学药物

目的:采用电喷雾-离子迁移谱(electrospray ionization-ion mobility spectrometry,ESI-IMS)技术,建立减肥类保健食品中非法添加的22种化学药品的现场快速检测方法。方法:样品经适量80%甲醇溶液超声提取获得供试品储备液,用含0.5%乙酸(V/V)的80%甲醇溶液适量稀释后,采用正离子模式(源电压:2200 V)检测普罗布考、盐酸芬氟拉明、盐酸安非他酮、盐酸吡格列酮、瑞格列奈、吉非罗齐、盐酸西布曲明、盐酸N-单去甲基西布曲明、盐酸N,N-双去甲基西布曲明、盐酸氟西汀、马来酸罗格列酮、盐酸伪麻黄碱、盐酸甲基安非他明、非诺贝特、吲达帕胺、比沙可啶、盐酸二甲双胍、酚酞。供试品储备液用含0.5%氨水(V/V)的80%甲醇溶液适量稀释,在负离子模式(源电压:1800 V)下检测呋塞米、氢氯噻嗪、氯噻嗪、氟伐他汀钠。迁移管电压均为8000 V,进气口温度和迁移管温度为180 ℃,门电压45 V,栅脉冲宽度120 μs。并用所建方法对40批市场抽查减肥类保健食品进行非法添加筛查。结果:该方法专属性良好,22种减肥类标准品迁移时间在8.0~16.3 ms之间,在基质样品中检出限为0.05~8.0 mg·L-1。样品中1批检出西布曲明,1批检出酚酞,1批检出氟西汀。结论:本方法迅速、灵敏,适用于减肥类保健食品中非法添加化学药品的快速筛查工作。     

液相色谱-离子阱质谱法同时测定减肥类保健食品中非法添加的12种化学药物

目的 建立减肥类保健食品中12种非法添加化学药物的高效液相色谱-离子阱质谱联用 分析方法,并对56批抽检样品进行检测。方法 样品经甲醇超声提取后,经SHISEIDO CAPCELL-PAK C18色谱柱（150 mm×4.6 mm,5 μm）分离,以乙酸铵溶液-甲醇为流动相,梯度洗脱。采用ESI离子源,正离子扫描模式,对样品中非法添加的12种化合物进行定性检测。结果 该法能够同时完成对保健食品中12种非法添加化学药物的检测,方法检出限为0.1~0.5 ng/mL。采用该法对56批抽检样品进行检验,其中13批检出西布曲明和N-单去甲基西布曲明,4批检出奥利司他,阳性检出率为30%。结论 该法专属性好、灵敏度高、简便快速,可用于减肥类保健食品中非法添加化学药物的快速筛查。     

UPLC-MS/MS法同时测定减肥食品中55种非法添加物

目的 建立超高效液相色谱-串联质谱同时测定减肥类食品中55种非法添加物的分析方法。方法 样品经甲醇超声提取后,采用Agilent Eclipse Plus C₁₈ RRHD色谱柱(2.1 mm×100 mm,1.8μm)分离,以乙腈-0.1%甲酸为流动相进行梯度洗脱。在正负离子扫描条件下,采用动态多反应监测模式监测。结果 55种非法添加药物在相应的线性范围内均呈现良好线性关系,相关系数大于0.995,平均回收率75.2%～121.6%,相对标准偏差<12%,各化学药物的检测限在0.02～1.25μg/g。应用该方法对50批样品进行了检测,其中有38批次样品检出托拉塞米、大黄素、西布曲明、N-单去甲基西布曲明、N,N-双去甲基西布曲明、比沙可啶、麻黄碱、甲基麻黄碱、氢氯噻嗪、氟西汀等非法添加物。结论 该方法简单、快速、灵敏、准确、高效,兼具定性定量检测的优点,可用于食品中减肥类化学药物的高通量检测。     

国家食药监局:哈药、九芝堂卷入“售假门”

<正>国家食药监局日前在官网公告称,在保健食品抽检中发现"赛而牌维美克减肥颗粒"等21种产品含有违禁化学药物成分,属于假冒保健食品,九芝堂和哈药集团现身"黑名单"。国家食药监局的曝光名单显示:包括赛而牌维美克减肥颗粒、蚁力神牌鸣琪胶囊、诺瑞特牌巴拿拿胶囊等多个产品,均被检出违禁化学药物成分,包括酚酞、西布曲明、格     

UPLC-Q/Orbitrap MS快速检测酵素产品中非法添加的7种减肥类药物

基于超高效液相色谱-四级杆/静电场轨道阱高分辨质谱(UPLC-Q/Orbitrap MS)建立了酵素食品中7种非法添加减肥类药物(西布曲明、N-单去甲基西布曲明、N,N-双去甲基西布曲明、芬氟拉明、麻黄碱、酚酞和呋塞米)的快速检测方法。样品采用乙腈提取,Hypersil Gold C_(18)色谱柱(100mm×2.1 mm,3μm)分离,正离子模式使用0.1%甲酸乙酸铵(5 mmol/L)和甲醇进行梯度洗脱,负离子模式使用乙酸铵(5 mmol/L)和甲醇进行梯度洗脱,流速0.2 mL/min,柱温30℃。呋塞米采用负离子模式扫描,其他化合物采用正离子模式扫描,结果表明,7种减肥类药物在(0.5~50.0)ng/mL范围内具有良好的线性(线性相关系数均大于0.999),各组分的检出限在(0.37~2.8)μg/kg之间,定量限在(1.2~9.4)μg/kg之间,回收率在90.1%~105.9%,精密度在1.5%~3.5%。该法具有准确、简单、快捷的特点,可为酵素产品及其他产品中7种非法添加减肥类药物的快速检测提供参考依据。     

Rapid screening of illicit additives in weight loss dietary supplements with desorption corona beam ionisation (DCBI) mass spectrometry

Desorption corona beam ionisation (DCBI), the relatively novel ambient mass spectrometry (MS) technique, was utilised to screen for illicit additives in weight-loss food. The five usually abused chemicals - fenfluramine, N-di-desmethyl sibutramine, N-mono-desmethyl sibutramine, sibutramine and phenolphthalein - were detected with the proposed DCBI-MS method. Fast single-sample and high-throughput analysis was demonstrated. Semi-quantification was accomplished based on peak areas in the ion chromatograms. Four illicit additives were identified and semi-quantified in commercial samples. As there was no tedious sample pre-treatment compared with conventional HPLC methods, high-throughput analysis was achieved with DCBI. The results proved that DCBI-MS is a powerful tool for the rapid screening of illicit additives in weight-loss dietary supplements.     

Rapid screening of illicit additives in weight loss dietary supplements with desorption corona beam ionisation (DCBI) mass spectrometry

Desorption corona beam ionisation (DCBI), the relatively novel ambient mass spectrometry (MS) technique, was utilised to screen for illicit additives in weight-loss food. The five usually abused chemicals – fenfluramine, N-di-desmethyl sibutramine, N-mono-desmethyl sibutramine, sibutramine and phenolphthalein – were detected with the proposed DCBI-MS method. Fast single-sample and high-throughput analysis was demonstrated. Semi-quantification was accomplished based on peak areas in the ion chromatograms. Four illicit additives were identified and semi-quantified in commercial samples. As there was no tedious sample pre-treatment compared with conventional HPLC methods, high-throughput analysis was achieved with DCBI. The results proved that DCBI-MS is a powerful tool for the rapid screening of illicit additives in weight-loss dietary supplements.     

Analysis of six synthetic adulterants in herbal weight-reducing dietary supplements by LC electrospray ionization-MS

A liquid chromatography-electrospray ionization-mass spectrometry (LC-ESI-MS) method was developed for the simultaneous determination of six synthetic adulterants, namely fenfluramine, phenolphthalein, N-di-desmethyl sibutramine, N-mono-desmethyl sibutramine, sibutramine, and orlistat. The method was applied to the analysis of herbal weight-reducing dietary supplements. Chromatographic separation of the analytes on a C(8) reversed-phase column was achieved using a gradient elution of solvent A: acetonitrile and solvent B: aqueous 20 mM ammonium formate solution. Sildenafil was utilized as an internal standard for quantification. The MS detector was operated in positive electrospray ionization mode. Selected-ion monitoring (SIM) was carried out for m/z 232, 319, 252, 266, 280, 496, and 475 for fenfluramine, phenolphthalein, N-di-desmethyl sibutramine, N-mono-desmethyl sibutramine, sibutramine, orlistat, and sildenafil, respectively. The method was validated for accuracy, precision, linearity, and selectivity. The limits of detection for the six synthetic adulterants ranged from 0.0018 to 0.73 microg g(-1). The proposed method was used for a small survey of 22 dietary supplements of which eleven samples were adulterated with phenolphthalein, N-mono-desmethyl sibutramine, and sibutramine at levels from 0.212 to 96.2 mg g(-1).     

Analysis of six synthetic adulterants in herbal weight-reducing dietary supplements by LC electrospray ionization-MS

A liquid chromatography-electrospray ionization-mass spectrometry (LC-ESI-MS) method was developed for the simultaneous determination of six synthetic adulterants, namely fenfluramine, phenolphthalein, N-di-desmethyl sibutramine, N-mono-desmethyl sibutramine, sibutramine, and orlistat. The method was applied to the analysis of herbal weight-reducing dietary supplements. Chromatographic separation of the analytes on a C₈ reversed-phase column was achieved using a gradient elution of solvent A: acetonitrile and solvent B: aqueous 20 mM ammonium formate solution. Sildenafil was utilized as an internal standard for quantification. The MS detector was operated in positive electrospray ionization mode. Selected-ion monitoring (SIM) was carried out for m/z 232, 319, 252, 266, 280, 496, and 475 for fenfluramine, phenolphthalein, N-di-desmethyl sibutramine, N-mono-desmethyl sibutramine, sibutramine, orlistat, and sildenafil, respectively. The method was validated for accuracy, precision, linearity, and selectivity. The limits of detection for the six synthetic adulterants ranged from 0.0018 to 0.73 µg g^?1. The proposed method was used for a small survey of 22 dietary supplements of which eleven samples were adulterated with phenolphthalein, N-mono-desmethyl sibutramine, and sibutramine at levels from 0.212 to 96.2 mg g^?1.     

Detection of hazardous weight-loss substances in adulterated slimming formulations using ultra-high-pressure liquid chromatography with diode-array detection

The presence on the market of illegal products for slimming purposes or the treatment of overweight is a public health issue. These products may contain illicit chemicals in order to improve their effectiveness. Some of these weight-loss compounds are responsible for adverse events, including fatal outcomes. A general strategy for the analysis of any suspect formulation begins with a large screening for the general search of a wide range of compounds. A methodology for the qualitative and quantitative determination of 34 compounds in slimming preparations (such as dietary supplements or medicinal products) was used for the control of slimming formulations from the market, including over the Internet. The fast liquid chromatography system (ultra-high-pressure liquid chromatography) used a gradient of solvent (phosphate buffer and acetonitrile), a C18 endcapped column and a diode array detector. This system allows dual identification based on retention time and UV spectra. The analytical method is simple, fast and selective since 34 weight-loss compounds can be detected in a 15-min run time. Thus, 32 commercial slimming formulations were analysed using this method, allowing the detection and quantification of hazardous active substances: caffeine, clenbuterol, nicotinamide, phenolphthalein, rimonabant, sibutramine, didesmethylsibutramine, synephrine and yohimbine.     

Detection of hazardous weight-loss substances in adulterated slimming formulations using ultra-high-pressure liquid chromatography with diode-array detection

The presence on the market of illegal products for slimming purposes or the treatment of overweight is a public health issue. These products may contain illicit chemicals in order to improve their effectiveness. Some of these weight-loss compounds are responsible for adverse events, including fatal outcomes. A general strategy for the analysis of any suspect formulation begins with a large screening for the general search of a wide range of compounds. A methodology for the qualitative and quantitative determination of 34 compounds in slimming preparations (such as dietary supplements or medicinal products) was used for the control of slimming formulations from the market, including over the Internet. The fast liquid chromatography system (ultra-high-pressure liquid chromatography) used a gradient of solvent (phosphate buffer and acetonitrile), a C18 endcapped column and a diode array detector. This system allows dual identification based on retention time and UV spectra. The analytical method is simple, fast and selective since 34 weight-loss compounds can be detected in a 15-min run time. Thus, 32 commercial slimming formulations were analysed using this method, allowing the detection and quantification of hazardous active substances: caffeine, clenbuterol, nicotinamide, phenolphthalein, rimonabant, sibutramine, didesmethylsibutramine, synephrine and yohimbine.     

Active pharmaceutical ingredients detected in herbal food supplements for weight loss sampled on the Dutch market

Herbal food supplements claiming to reduce weight may contain active pharmacological ingredients (APIs) that can be used for the treatment of overweight and obesity. The aim of this study was to determine whether herbal food supplements for weight loss on the Dutch market contain APIs with weight loss properties. Herbal food supplements intended for weight loss (n = 50) were sampled from August 2004 to May 2013. An HPLC-DAD-MS/MS method was used to screen for the presence of the APIs in herbal supplements. In 24 samples the APIs sibutramine, desmethylsibutramine (DMS), didesmethylsibutramine (DDMS), rimonabant, sildenafil and/or the laxative phenolphthalein were identified 41 times. The presence of these APIs was, however, not stated on the label. The potential pharmacological effects of the detected APIs were estimated using data from reported effective doses of approved drugs. Use of 20 of the 24 herbal food supplements may result in potential pharmacological effects. Furthermore, risk assessment of phenolphthalein, a suspected carcinogen and found to be present in 10 supplements, based on the margin of exposure (MOE) approach, resulted in MOE values of 96–30 000. MOE values lower than 10 000 (96–220) were calculated for the daily intake levels of four out of these 10 supplements in which phenolphthalein was found. However, taking into account that weight loss preparations may be used for only a few weeks or months rather than during a lifetime, MOE values may be two to three orders of magnitude higher. The current study shows that the use of food supplements with sibutramine, DMS, DDMS and/or phenolphthalein could result in pharmacological effects.