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首页> 外文期刊>Journal of separation science. >A reliable isotope dilution method for simultaneous determination of fumonisins B1, B2 and B3 in traditional Chinese medicines by ultra-high-performance liquid chromatography-tandem mass spectrometry
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A reliable isotope dilution method for simultaneous determination of fumonisins B1, B2 and B3 in traditional Chinese medicines by ultra-high-performance liquid chromatography-tandem mass spectrometry

机译：超高效液相色谱-串联质谱法同时测定中药中伏马毒素B1，B2和B3的可靠同位素稀释方法

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摘要

A reliable isotope dilution method for simultaneous determination of fumonisin B1, fumonisin B2 and fumonisin B3 in traditional Chinese medicines by ultra-high-performance LC-MS/MS was developed, and a special focus was placed on the optimization of extraction, cleanup, ultra-high-performance LC separation and MS/MS conditions. Homogenized samples were extracted by 50% acetonitrile aqueous solution and purified with MultiSep 211 Fum columns. A linear gradient mobile phase, consisting of water containing 0.2% formic acid and acetonitrile/methanol (50:50 v/v) and an Acquity UPLC HSS T3 column (100 mm x 2.1 mm, 1.8 μm) were employed to obtain the best resolution of the analytes for the positive ESI~+ analysis. The established method was validated by determining the linearity (R~2≥0.9991), sensitivity (LOQ, 0.08-0.16 ng/mL), recovery (88.2-113.3%) and precision (RSD≤12.3%). Finally, the validated method was successfully applied to the determination of fumonisins in different traditional Chinese medicines. Of 35 samples, 18 were contaminated with fumonisins. The mean levels (incidence) of fumonisin B1, fumonisin B1 and fumonisin B1 in positive samples were 8.55 (94.4%), 4.88 (77.8%) and 0.52 mg/kg (33.3%), respectively. Based on the contaminant situations, a possible association between the contamination levels and the selected herbs was clarified in this study.
机译：建立了一种可靠的同位素稀释方法，通过超高效液相色谱/质谱联用同时测定中药中的伏马毒素B1，伏马毒素B2和伏马毒素B3，并着重于提取，纯化，超滤的优化。 -高效液相色谱分离和MS / MS条件。均质的样品用50％乙腈水溶液萃取，并用MultiSep 211 Fum色谱柱纯化。使用由0.2％甲酸和乙腈/甲醇（50:50 v / v）组成的线性梯度流动相和Acquity UPLC HSS T3色谱柱（100 mm x 2.1 mm，1.8μm）获得最佳分离度进行正ESI〜+分析的分析物。通过测定线性（R〜2≥0.9991），灵敏度（LOQ，0.08-0.16 ng / mL），回收率（88.2-113.3％）和精密度（RSD≤12.3％）来验证所建立的方法。最后，验证方法成功地用于不同中药中伏马毒素的测定。在35个样本中，有18个被伏马菌素污染。阳性样品中伏马毒素B1，伏马毒素B1和伏马毒素B1的平均水平（发生率）分别为8.55（94.4％），4.88（77.8％）和0.52 mg / kg（33.3％）。根据污染情况，在这项研究中阐明了污染水平与所选草药之间的可能联系。

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