PDF(Pubmed)
Abstract：
Patulin, a toxic mycotoxin, can contaminate apple-derived products. The FDA has established an action level of 50 ppb (ng/g) for patulin in apple juice and apple juice products. To effectively monitor this mycotoxin, there is a need for adequate analytical methods that can reliably and efficiently determine patulin levels. In this work, we developed an automated sample preparation workflow followed by liquid chromatography-atmospheric pressure chemical ionization tandem mass spectrometry (LC-APCI-MS/MS) detection to identify and quantify patulin in a single method, further expanding testing capabilities for monitoring patulin in foods compared to traditional optical methods. Using a robotic sample preparation system, apple juice, apple cider, apple puree, apple-based baby food, applesauce, fruit rolls, and fruit jam were fortified with 13C-patulin and extracted using dichloromethane (DCM) without human intervention, followed by an LC-APCI-MS/MS analysis in negative ionization mode. The method achieved a limit of quantification of 4.0 ng/g and linearity ranging from 2 to 1000 ng/mL (r2 > 0.99). Quantitation was performed with isotope dilution using 13C-patulin as an internal standard and solvent calibration standards. Average recoveries (relative standard deviations, RSD%) in seven spike matrices were 95% (9%) at 10 ng/g, 110% (5%) at 50 ng/g, 101% (7%) at 200 ng/g, and 104% (4%) at 1000 ng/g (n = 28). The ranges of within-matrix and between-matrix variability (RSD) were 3-8% and 4-9%, respectively. In incurred samples, the identity of patulin was further confirmed with a comparison of the information-dependent acquisition-enhanced product ion (IDA-EPI) MS/MS spectra to a reference standard. The metrological traceability of the patulin measurements in an incurred apple cider (21.1 ± 8.0 µg/g) and apple juice concentrate (56.6 ± 15.6 µg/g) was established using a certified reference material and calibration data to demonstrate data confidence intervals (k = 2, 95% confidence interval).
摘要：
棒曲霉素,一种有毒的霉菌毒素,会污染苹果衍生产品。FDA已经确定苹果汁和苹果汁产品中的棒曲霉素的作用水平为50ppb(ng/g)。为了有效监测这种霉菌毒素，需要能够可靠且有效地测定棒曲霉素水平的适当的分析方法。在这项工作中,我们开发了一种自动样品制备工作流程，然后进行液相色谱-大气压化学电离串联质谱（LC-APCI-MS/MS）检测，以在单一方法中鉴定和定量棒曲霉素，与传统的光学方法相比，进一步扩大了监测食品中棒曲霉素的测试能力。使用机器人样品制备系统，苹果汁,苹果酒,苹果泥,以苹果为基础的婴儿食品，苹果酱,水果卷,和果酱用13C-棒曲霉素强化，并用二氯甲烷（DCM）萃取，无需人工干预，然后进行负电离模式的LC-APCI-MS/MS分析。该方法实现了4.0ng/g的定量限，线性范围为2至1000ng/mL（r2>0.99）。使用13C-棒曲霉素作为内标和溶剂校准标准,用同位素稀释进行定量。平均回收率(相对标准偏差，在10ng/g时，七个刺突基质中的RSD％）为95％（9％），在50ng/g时110%(5%)，200ng/g时101%(7%)，和104%(4%)在1000ng/g(n=28)。矩阵内和矩阵间变异性（RSD）的范围为3-8％和4-9％，分别。在招致的样品中，通过将信息依赖性采集增强产物离子(IDA-EPI)MS/MS光谱与参比标准品进行比较,进一步证实了棒曲霉素的身份.使用经过认证的参考材料和校准数据来证明数据置信区间（k=2，95％置信区间），建立了发生的苹果酒（21.1±8.0µg/g）和苹果汁浓缩物（56.6±15.6µg/g）中的棒曲霉素测量的计量可追溯性。
