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A rapid ion chromatography column-switching method for online sample pretreatment and determination of L-carnitine, choline and mineral ions in milk and powdered infant formula

机译:在线样品前处理和测定婴儿奶粉和奶粉中的左旋肉碱,胆碱和矿物质离子的快速离子色谱柱切换方法

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A simple and rapid column-switching ion chromatography with non-suppressed conductivity detection method was developed for simultaneous determination of L-carnitine, choline and mineral ions (free sodium, potassium, magnesium and calcium ions) in milk and powdered infant formula samples. On-line sample clean-up was achieved on the pretreatment column Dionex IonPac NG1 (50 mm × 4 mm, i.d.), with pretreatment elution (3 mmol L?1 MSA) and washing solution (100% acetonitrile) at a flow rate of 1.0 mL min?1. After column switching, the separation and determination of analytes were performed using guard column Dionex IonPac SGS (50 mm × 4 mm, i.d.) and analytical column Dionex IonPac SCS (250 mm × 4 mm, i.d.) with an isocratic mobile phase consisting of 3 mmol L?1 MSA and 10% (v/v) acetonitrile, at flow-rate of 1 mL min?1, followed by non-suppressed conductivity detection. The organic matrices clean-up performance of the proposed method was studied using an UV detector working at 200–400 nm. Under the optimal conditions, detection limits (S/N = 3) ranging from 0.05–0.30 mg L?1, good linearities in the range of 1–100 mg L?1 with a correlation coefficient over 0.9973, and satisfactory recoveries in the range between 94% and 105% with relative standard deviation less than 2.1% for real samples were attainted. The proposed method was successfully applied to rapid, simultaneous, and labour-saving detection of L-carnitine, choline, and mineral ions in milk and powdered infant formula samples.
机译:建立了一种非抑制电导率检测方法的快速简便的柱切换离子色谱法,用于同时测定牛奶中的 L 肉毒碱,胆碱和矿物质离子(游离钠,钾,镁和钙离子)和婴儿配方奶粉样品。在预处理柱Dionex IonPac NG1(50 mm×4 mm,id)上进行在线样品净化,并进行预处理洗脱(3 mmol L ?1 MSA )和洗涤液(100%乙腈),流速为1.0 mL min ?1 。更换色谱柱后,使用保护柱Dionex IonPac SGS(50 mm×4 mm,id)和分析柱Dionex IonPac SCS(250 mm×4 mm,id)进行分离和测定分析物,等度流动相为3 mmol L ?1 MSA和10%(v / v)乙腈,流速为1 mL min ?1 < / small>,然后进行非抑制的电导率检测。使用工作在200-400 nm的紫外检测器研究了所提出方法的有机基质净化性能。在最佳条件下,检出限(S / N = 3)范围为0.05–0.30 mg L ?1 ,线性范围为1–100 mg L < small> ?1 ,相关系数超过0.9973,对真实样品的回收率在94%到105%之间,相对标准偏差小于2.1%。该方法成功地应用于牛奶和婴儿配方奶粉样品中的 L -肉碱,胆碱和矿物质离子的快速,同时和省力的检测。

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