LC-MS/MS测定膳食补充剂中壳聚糖分析方法的建立

Ji Eun Park, M. Oh
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引用次数: 0

摘要

食品药品安全处正在修改膳食补充剂(功能性保健食品)的检验方法,以建立韩国的管理标准和规范。在本研究中,我们开发了分析测试方法,以提高壳聚糖测试方法的灵敏度和选择性。采用液相色谱-串联质谱法对壳聚糖酸水解制备葡萄糖胺进行分析。该方法可用于表征和定量含壳聚糖的膳食补充剂制剂。方法在78 ~ 2500 ng/mL范围内有效,标准校准曲线呈线性关系,决定系数(r²)> 0.999。检测限为51 ng/mL,定量限为154 ng/mL。3种浓度下加样回收率为94.8 ~ 102.9%,相对标准偏差小于3.1%,精密度为0.8 ~ 2.5%。这些符合既定的验证标准(官方分析化学家协会)。本研究为修订《保健功能食品规范》中壳聚糖检测方法提供了科学依据。
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Analytical Method Development for Determination of Chitosan by LC-MS/MS in Dietary Supplement
The Ministry of Food and Drug Safety is amending its test methods for dietary supplements (functional health food) to establish regulatory standards and specifications in South Korea. In this study, we develop analytical test methods to improve the sensitivity and selectivity of the chitosan test method. We develop liquid chromatographic-tandem mass spectrometry for a chitosan analysis using acid hydrolysis to glucosamine. This method can be used to characterize and quantify dietary supplement formulations containing chitosan. The procedure was validated in the 78 ~ 2,500 ng/mL range, and standard calibration curves presented linearity with the coefficient of determination (r²) > 0.999. The limits of detection and quantitation were 51 ng/mL and 154 ng/mL, respectively. The recovery results ranged between 94.8 ~ 102.9% at three different concentration levels with relative standard deviations less than 3.1%, and precision (0.8 ~ 2.5%) was obtained. These are in accordance with the established validation criteria (Association of Official Analytical Chemists). Subsequently, our research provides scientific evidence for amending the chitosan test method for the Health Functional Food Codes.
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