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Generic and rapid determination of low molecular weight organic chemical contaminants in protein powder by using ultra-performance liquid chromatography-tandem mass spectrometry
Journal of Chromatography B ( IF 3 ) Pub Date : 2020-01-03 , DOI: 10.1016/j.jchromb.2020.121967
Jia Zhan , Xi-zhi Shi , Xu-wen Xu , Guo-zhou Cao , Xian-feng Chen

A rapid, simple, and generic analytical method that could simultaneously determine 291 undesirable low molecular weight chemical contaminants from different drug families in protein powder, such as veterinary drugs and pesticides, etc, had been developed. This method comprised the extraction with acetonitrile-dimethyl sulfoxide (DMSO), clean-up through dispersive solid phase extraction (D-SPE) and low temperature filtration, and analysis by ultra-performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry at multiple-reaction monitoring mode. Acetonitrile-DMSO was more generic than acetonitrile or methanol for the extraction of large-scale organic chemical contaminants with different polarities in protein powder. Most interferences in the extract were eliminated by the combination of D-SPE and low temperature filtration, which simultaneously provided satisfactory recoveries of both hydrophobic and hydrophilic analytes. In particular, besides the purification function, the sorbent of D-SPE also played an important role in grinding samples to improve extraction efficiency during homogenization. This streamlined approach allowed the processes of extraction and the main purification were carried out in one-step, and dramatically reduced sample preparation turnaround times and solvent consumption. For quantification, matrix-fortified calibration curves showed competent linearity for most of the target compounds with linear regression coefficients (r) higher than 0.9900, except for two analytes. The limits of quantification ranged from 0.1 μg/kg to 50 μg/kg, which was usually sufficient to verify the compliance of products with legal tolerances. The average recoveries for spiked protein powder ranged from 65.6% to 142.2% with associated RSD values between 0.5% and 28.5%. For over 90% of the analytes, the recoveries were between 70% and 120% with RSD values in the range of 1%–15%. Applying this method in routine monitoring programs would drastically reduce both effort and time.



中文翻译:

超高效液相色谱-串联质谱法通用快速测定蛋白粉中的低分子量有机化学污染物

已经开发出一种快速,简单且通用的分析方法,该方法可以同时确定291种来自蛋白质粉中不同药物家族的低分子量化学污染物,例如兽药和农药等。该方法包括乙腈-二甲基亚砜(DMSO)萃取,分散固相萃取(D-SPE)和低温过滤净化,以及超高效液相色谱与电喷雾电离串联质谱联用进行多级分析。反应监控模式。乙腈-D​​MSO比乙腈或甲醇更通用,可用于提取蛋白质粉末中极性不同的大规模有机化学污染物。D-SPE和低温过滤的结合消除了萃取物中的大多数干扰,同时提供了令人满意的疏水性和亲水性分析物回收率。特别是,除纯化功能外,D-SPE的吸附剂在研磨样品中也起着重要作用,以提高均质过程中的提取效率。这种简化的方法允许一步一步进行提取和主要纯化过程,并大大减少了样品制备的周转时间和溶剂消耗。为了定量,除两种分析物外,基质强化的校准曲线对大多数目标化合物显示出满意的线性,线性回归系数(r)高于0.9900。定量限为0.1μg/ kg至50μg/ kg,通常足以验证产品是否符合法律规定的公差。加标蛋白粉的平均回收率在65.6%至142.2%之间,相关的RSD值在0.5%至28.5%之间。对于90%以上的分析物,回收率在70%至120%之间,RSD值在1%至15%的范围内。在常规监视程序中应用此方法将大大减少工作量和时间。

更新日期:2020-01-04
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