College of Pharmaceutical Sciences, Zhejiang University, Hangzhou, P. R. China.
J Sep Sci. 2010 Jul;33(13):1923-32. doi: 10.1002/jssc.201000094.
A speedy and selective ultra-HPLC-MS/MS method for simultaneous determination of deoxynivalenol (DON), 3-acetyldeoxynivalenol (3-ADON), 15-ADON, nivalenol and fusarenon X in traditional Chinese medicines (TCMs) was developed. The method was based on one-step sample cleanup using reliable homemade cleanup cartridges. A linear gradient mobile-phase system, consisting of water containing 0.2% aqueous ammonia and acetonitrile/methanol (90:10, v/v) at a flow rate of 0.4 mL/min, and an Acquity UPLC HSS T3 column (100 mm x 2.1 mm, 1.8 microm) were employed to obtain the best resolution of the target analytes. [(13)C(15)]-DON was used as the internal standard to accomplish as accurate as possible quantitation. The established method was further validated by determining the linearity (R(2) > or = 0.9990), sensitivity (LOQ, 0.29-0.99 microg/kg), recovery (88.5-119.5%) and precision (RSD < or = 15.8%). It was shown to be a suitable method for simultaneous determination of DON, 3-ADON, 15-ADON, nivalenol and fusarenon X in various TCM matrices. The utility and practical impact of the method was demonstrated using different TCM samples.
建立了同时测定中药中脱氧雪腐镰刀菌烯醇（DON）、3-乙酰脱氧雪腐镰刀菌烯醇（3-ADON）、15-乙酰脱氧雪腐镰刀菌烯醇（15-ADON）、雪腐镰刀菌烯醇和伏马菌素 X 的超快速、高选择性的 UPLC-MS/MS 方法。该方法基于一步样品净化，采用可靠的自制净化小柱。在流速为 0.4 mL/min 时，采用水（含 0.2%氨水）-乙腈/甲醇（90:10，v/v）线性梯度洗脱体系，在 Acquity UPLC HSS T3 柱（100 mm×2.1 mm，1.8 µm）上获得了目标分析物的最佳分离度。[(13)C(15)]-DON 被用作内标，以尽可能准确地进行定量。通过测定线性（R(2)≥0.9990）、灵敏度（LOQ，0.29-0.99 µg/kg）、回收率（88.5%-119.5%）和精密度（RSD≤15.8%）对所建立的方法进行了进一步验证。该方法适用于同时测定各种中药基质中的 DON、3-ADON、15-ADON、雪腐镰刀菌烯醇和伏马菌素 X。并通过不同的中药样品验证了该方法的实用性和实际影响。
