{"title":"LC-MS/MS测定膳食补充剂中壳聚糖分析方法的建立","authors":"Ji Eun Park, M. Oh","doi":"10.17480/psk.2022.66.4.204","DOIUrl":null,"url":null,"abstract":"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.","PeriodicalId":23923,"journal":{"name":"Yakhak Hoeji","volume":"22 1","pages":""},"PeriodicalIF":0.0000,"publicationDate":"2022-08-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Analytical Method Development for Determination of Chitosan by LC-MS/MS in Dietary Supplement\",\"authors\":\"Ji Eun Park, M. Oh\",\"doi\":\"10.17480/psk.2022.66.4.204\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"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.\",\"PeriodicalId\":23923,\"journal\":{\"name\":\"Yakhak Hoeji\",\"volume\":\"22 1\",\"pages\":\"\"},\"PeriodicalIF\":0.0000,\"publicationDate\":\"2022-08-30\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Yakhak Hoeji\",\"FirstCategoryId\":\"1085\",\"ListUrlMain\":\"https://doi.org/10.17480/psk.2022.66.4.204\",\"RegionNum\":0,\"RegionCategory\":null,\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"\",\"JCRName\":\"\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Yakhak Hoeji","FirstCategoryId":"1085","ListUrlMain":"https://doi.org/10.17480/psk.2022.66.4.204","RegionNum":0,"RegionCategory":null,"ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"","JCRName":"","Score":null,"Total":0}
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.