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采用超高效液相色谱-串联质谱法定量测定水溶液中壳聚糖的新方法。

A novel method to quantify chitosan in aqueous solutions by ultrahigh-performance liquid chromatography-tandem mass spectrometry.

机构信息

Beijing Institute of Radiation Medicine, Beijing 100850, China.

Beijing Institute of Radiation Medicine, Beijing 100850, China.

出版信息

Carbohydr Polym. 2024 Apr 1;329:121758. doi: 10.1016/j.carbpol.2023.121758. Epub 2024 Jan 2.

DOI:10.1016/j.carbpol.2023.121758
PMID:38286539
Abstract

In this study, a novel and accurate quantitative analysis method for the direct determination of chitosan (CS) in aqueous solutions using ultrahigh-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) is presented. By detecting the mass spectrum response intensity of a series of CS characteristic ion pairs, the sample concentration (abscissa) was linearly fitted with the total ion current (TIC) response intensity of its characteristic ion pairs (ordinate). A reliable standard curve was derived for quantifying CS in the range of 125-4000 ng/mL. Under the detection conditions, this CS quantification method yielded acceptable specificity (no interference peak), linearity (with correlation coefficient (r) values >0.999), precision (acceptable limit RSD < 3 %, RSD < 6 %), accuracy (RE within the acceptable limits of ±5 %), and stability (acceptable limit RE within ±5 %, RSD < 3 %). Moreover, the applicability of measurement was verified when a series of substrates did not interact with CS in the solution. Results have verified the applicability of this method for determining CS content in different composites. This study provides a method for determining CS content with significant practical value and economic benefit.

摘要

本研究提出了一种新颖且准确的定量分析方法,可通过超高效液相色谱-串联质谱法(UPLC-MS/MS)直接测定水溶液中的壳聚糖(CS)。通过检测一系列 CS 特征离子对的质谱响应强度,将样品浓度(横坐标)与特征离子对的总离子流(TIC)响应强度(纵坐标)进行线性拟合。得出了一种可靠的标准曲线,用于在 125-4000ng/mL 范围内定量 CS。在检测条件下,该 CS 定量方法具有可接受的特异性(无干扰峰)、线性(相关系数(r)值>0.999)、精密度(可接受的 RSD<3%,RSD<6%)、准确度(RE 在可接受的±5%范围内)和稳定性(RE 在可接受的±5%范围内,RSD<3%)。此外,当一系列基质在溶液中不与 CS 相互作用时,验证了测量的适用性。结果验证了该方法在测定不同复合材料中 CS 含量的适用性。本研究提供了一种具有显著实用价值和经济效益的 CS 含量测定方法。

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