In this paper, an ultra-high-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (UHPLC-Q-TOF HRMS) method was developed and validated for screening, confirmation and quantitation of 31 anti-impotence compounds potentially illegally added to herbal-based dietary supplements. The analytes were well separated by the mobile phase consisted of 0.1% formic acid solution and acetonitrile with gradient elution at a flow rate of 0.3 mL/min. The MS analysis was operated in positive mode and the mass error of the 31 compounds were below 2.9 ppm. The method validation showed good linearity with coefficients of determination (r2) higher than 0.9973 for all analytes. LODs and LLOQs ranged from 0.005 to 0.50 μg/g or μg /mL and from 0.02 to 1.24 μg /g or μg/mL, respectively. The accuracy was in the range of 86.6% to 113.7%, while the intra-and inter-day precision were in the ranges of 0.9-7.6% and 0.9-11.4%, respectively. The absolute and relative matrix effect were in the range of 65.8-115.6% and 0.6-13.3%. The mean recoveries were in the range of 80.5-116.9%. The stability ranged from 0.4% to 8.5%. Among 200 batches of herbal-based dietary supplements, sildenafil and/or tadalafil were found to be added illegally in two samples, while not very high concentration of icariin was detected in one sample. The Q-TOF mass spectrometry has been proved to be a very powerful and efficient tool for rapid screening of 31 anti-impotence compounds potentially illegally added to herbal-based dietary supplements, ensuring food safety and public health.

中文翻译：

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通过超高效液相色谱与四极杆飞行时间质谱联用同时分析可能​​非法添加到基于草药的膳食补充剂中的31种抗阳im化合物。

本文开发了一种结合四极杆飞行时间质谱（UHPLC-Q-TOF HRMS）的超高效液相色谱方法，并经过验证可用于筛查，确证和定量分析可能非法添加的31种抗功效化合物以草药为主的膳食补充剂。流动相由0.1％甲酸溶液和乙腈组成的流动相以0.3 mL / min的流速进行梯度洗脱，从而很好地分离了分析物。MS分析以阳性模式进行，这31种化合物的质量误差低于2.9 ppm。方法验证显示出良好的线性，所有分析物的测定系数（r2）均高于0.9973。LOD和LLOQ的范围分别为0.005至0.50μg/ g或μg/ mL和0.02至1.24μg/ g或μg/ mL。准确度在86.6％至113.7％之间，而日内和日间精度分别在0.9-7.6％和0.9-11.4％的范围内。绝对和相对基质效应在65.8-115.6％和0.6-13.3％的范围内。平均回收率在80.5-116.9％的范围内。稳定性为0.4％至8.5％。在200批次的基于草药的膳食补充剂中，发现在两个样品中非法添加了西地那非和/或他达拉非，而在一个样品中未检测到非常高的大麻素浓度。事实证明，Q-TOF质谱仪是一种非常有效的工具，可以快速筛查可能非法添加到基于草药的膳食补充剂中的31种抗阳im化合物，从而确保食品安全和公共健康。绝对和相对基质效应在65.8-115.6％和0.6-13.3％的范围内。平均回收率在80.5-116.9％的范围内。稳定性为0.4％至8.5％。在200批次的基于草药的膳食补充剂中，发现在两个样品中非法添加了西地那非和/或他达拉非，而在一个样品中未检测到非常高的大麻素浓度。事实证明，Q-TOF质谱仪是一种非常有效的工具，可快速筛查可能非法添加到基于草药的膳食补充剂中的31种抗阳pot化合物，从而确保食品安全和公共健康。绝对和相对基质效应在65.8-115.6％和0.6-13.3％的范围内。平均回收率在80.5-116.9％的范围内。稳定性为0.4％至8.5％。在200批次的基于草药的膳食补充剂中，发现在两个样品中非法添加了西地那非和/或他达拉非，而在一个样品中未检测到非常高的大麻素浓度。事实证明，Q-TOF质谱仪是一种非常有效的工具，可快速筛查可能非法添加到基于草药的膳食补充剂中的31种抗阳pot化合物，从而确保食品安全和公共健康。西地那非和/或他达拉非被发现在两个样品中被非法添加，而在一个样品中未检测到很高的大麻素浓度。事实证明，Q-TOF质谱仪是一种非常有效的工具，可快速筛查可能非法添加到基于草药的膳食补充剂中的31种抗阳pot化合物，从而确保食品安全和公共健康。西地那非和/或他达拉非被发现在两个样品中被非法添加，而在一个样品中未检测到很高的大麻素浓度。事实证明，Q-TOF质谱仪是一种非常有效的工具，可快速筛查可能非法添加到基于草药的膳食补充剂中的31种抗阳pot化合物，从而确保食品安全和公共健康。