College of Pharmaceutical Sciences, Zhejiang University, Hangzhou, P. R. China.
J Sep Sci. 2010 Sep;33(17-18):2723-33. doi: 10.1002/jssc.201000423.
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×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 μg/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.
建立了超高效液相色谱-串联质谱法同时测定中药中伏马菌素 B1、B2 和 B3 的可靠同位素稀释法，特别关注提取、净化、超高效液相色谱分离和 MS/MS 条件的优化。将均匀化的样品用 50%乙腈水溶液提取，用 MultiSep 211 Fum 柱净化。采用含 0.2%甲酸的水和乙腈/甲醇（50:50 v/v）的线性梯度流动相，以及 Acquity UPLC HSS T3 柱（100 mm×2.1 mm，1.8 μm），获得了最佳的分析物正电喷雾（+）分析分辨率。通过确定线性（R²≥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%）对建立的方法进行了验证。最后，将验证的方法成功应用于不同中药中伏马菌素的测定。在 35 个样品中，有 18 个受到伏马菌素的污染。阳性样品中伏马菌素 B1、B2 和 B3 的平均含量（检出率）分别为 8.55（94.4%）、4.88（77.8%）和 0.52 μg/kg（33.3%）。根据污染情况，本研究明确了污染水平与所选草药之间的可能关联。
