Article(id=1153429499640271159, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1153429493357203682, articleNumber=null, orderNo=null, doi=10.19812/j.cnki.jfsq11-5956/ts.20241114002, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1731513600000, receivedDateStr=2024-11-14, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1752928622398, onlineDateStr=2025-07-19, pubDate=1741968000000, pubDateStr=2025-03-15, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1752928622398, onlineIssueDateStr=2025-07-19, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1752928622398, creator=13701087609, updateTime=1752928622398, updator=13701087609, issue=Issue{id=1153429493357203682, tenantId=1146029695717560320, journalId=1149652044408987649, year='2025', volume='16', issue='5', pageStart='1', pageEnd='326', issueExtLink='null', onlineDate='null', pubDate='1741968000000', pubDateStr='2025-03-15', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=0, createTime=1752928620900, creator='13701087609', updateTime=1758690311058, updator='13701087609', preIssue=null, nextIssue=null, articleTotal=null, ext={EN=IssueExt(id=1177595773500932351, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1153429493357203682, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1177595773500932352, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1153429493357203682, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null, downloadFileDto=null}, startPage=32, endPage=37, ext={EN=ArticleExt(id=1153429500202307907, articleId=1153429499640271159, tenantId=1146029695717560320, journalId=1149652044408987649, language=EN, title=Determination of 4 kinds of breast milk oligosaccharides in milk powder by liquid chromatography-fluorescence method, columnId=1153429494888129034, journalTitle=Journal of Food Safety & Quality, columnName=Highlight: Guangzhou Inspection Testing and Certification Group Co., Ltd., runingTitle=null, highlight=null, articleAbstract=
Objective To establish a method for simultaneous determination the content of 4 kinds of human milk oligosaccharides [2'--fucosyllactose (2'-FL), 3'-sialic acid (3'-SL), 6'-sialic acid (6'-SL) and lactose-N-neotetraose (LNnT)] in milk powder by liquid chromatography-fluorescence method. Methods The samples were dissolved in water, enzymolized with amyloglucosidase or β-galactosidase, derived with 2-aminobenzamide (2-AB) and 2-methylpyridine borane (2-PB), and separated by amide bonding column, detected by fluorescence detector, and quantitated by internal standard methods. Results The 4 kinds of milk oligosaccharides had a good linear relationship in the concentration range of 10-600 μg/mL, and the correlation coefficients (r2) were more than 0.999. The limits of detection and quantification of 4 kinds of milk oligosaccharides were 0.94-2.31 mg/100 g and 3.12-7.69 mg/100 g, respectively; the recovery rates of 4 kinds of milk oligosaccharides were 97.7%-101.5%, and the relative standard deviations (RSD) (n=7) were 0.53%-3.09%. Conclusion This method does not have high requirements for people, equipments and environment for determining the content of 4 kinds of milk oligosaccharides in milk powder. The pre-treatment operation is simple, and it has good accuracy and precision. It can provide a reference for the quality control method of human milk oligosaccharides in milk powder.
, authors=null, authorsList=Si-Yi DENG, Wei-Qian HUANG, Jun-Fa WU, Tian-Fu QIN, Zu-Jian CHEN, Zi-Heng YU, Zhen-Jie LI, authorCompany=null, correspAuthors=Si-Yi DENG, authorNote=null, correspAuthorsNote=null, copyrightStatement=null, copyrightOwner=null, extLink=null, articleAbsUrl=null, sourceXml=null, magXml=null, pdfUrl=null, pdf=null, pdfFileSize=null, pdfExtLink=null, richHtmlUrl=null, mobilePdfUrl=null, reviewReport=null, pdfFirstPage=null, abstractGraph=null, abstractGraphContent=null, abstractVideo=null, citation=null, cebUrl=null, magXmlContent=null, mapNumber=null, fund=null), CN=ArticleExt(id=1153429525636567945, articleId=1153429499640271159, tenantId=1146029695717560320, journalId=1149652044408987649, language=CN, title=液相色谱-荧光法测定乳粉中4种母乳低聚糖, columnId=1153429495039123980, journalTitle=食品安全质量检测学报, columnName=本期重点：广州检验检测认证集团有限公司, runingTitle=null, highlight=null, articleAbstract=
目的 建立液相色谱-荧光法同时测定乳粉中4种母乳低聚糖[2'-岩藻糖基乳糖(2'-fucosyllactose, 2'-FL)、3'-唾液酸乳糖(3'-sialyllactose, 3'-SL)、6'-唾液酸乳糖(6'-sialyllactose, 6'-SL)和乳糖-N-新四糖(lacto-N-neo-tetraose, LNnT)]的含量分析方法。方法 样品加水溶解后, 使用淀粉葡萄糖苷酶或和β-半乳糖苷酶酶解, 用2-氨基苯甲酰胺(2-aminobenzamide, 2-AB)和2-甲基吡啶硼烷(2-methylpyridine borane, 2-PB)衍生后, 采用酰胺键合色谱柱分离, 荧光检测器检测和内标法定量。结果 4种母乳低聚糖在10~600 µg/mL质量浓度范围均有良好的线性关系, 相关系数均为r2>0.999; 4种母乳低聚糖的检出限和定量限分别为0.94~2.31 mg/100 g、3.12~7.69 mg/100 g; 4种母乳低聚糖加标回收率为97.7%~101.5%, 相对标准偏差(relative standard deviation, RSD) (n=7)为0.53%~3.09%。结论 该方法对测定乳粉中的4种母乳低聚糖含量的检测人员、设备和环境要求不高、前处理操作简单, 且具有良好的准确度和精密度, 可为乳粉中母乳低聚糖质量控制提供方法参考。
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Chromatograms of 4 kinds of standard solutions of human milk oligosaccharides, figureFileSmall=aJSUqOqmQmesNjPcH4ksnw==, figureFileBig=tAPhTE1IOGyANAq3LRN94A==, tableContent=null), ArticleFig(id=1177619526016446944, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153429499640271159, language=CN, label=图1, caption=
4种母乳低聚糖标准溶液色谱图, figureFileSmall=aJSUqOqmQmesNjPcH4ksnw==, figureFileBig=tAPhTE1IOGyANAq3LRN94A==, tableContent=null), ArticleFig(id=1177619526070972897, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153429499640271159, language=EN, label=Fig.2, caption=
Chromatogram of blank sample, figureFileSmall=CzCu6cUdMVOxGq1MDchklA==, figureFileBig=BJm+OmbbZJ+KJMgBMG+G/w==, tableContent=null), ArticleFig(id=1177619526163247586, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153429499640271159, language=CN, label=图2, caption=
空白样品色谱图, figureFileSmall=CzCu6cUdMVOxGq1MDchklA==, figureFileBig=BJm+OmbbZJ+KJMgBMG+G/w==, tableContent=null), ArticleFig(id=1177619526217773539, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153429499640271159, language=EN, label=Fig.3, caption=
Negative matrix adding standard solution (2'-FL, 3'-SL, 6'-SL) chromatogram, figureFileSmall=Uw6pxTsPRAWzKQs5VYyTsQ==, figureFileBig=DZ5liuKqR6Q0fUNlJEpo0g==, tableContent=null), ArticleFig(id=1177619526268105188, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153429499640271159, language=CN, label=图3, caption=
阴性基底粉加标(2'-FL、3'-SL、6'-SL)色谱图, figureFileSmall=Uw6pxTsPRAWzKQs5VYyTsQ==, figureFileBig=DZ5liuKqR6Q0fUNlJEpo0g==, tableContent=null), ArticleFig(id=1177619526335214053, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153429499640271159, language=EN, label=Fig.4, caption=
Chromatogram of negative matrix adding standard solution (LNnT), figureFileSmall=Fe5H1rH9RUoy7n9coXHWlQ==, figureFileBig=TLzCU3/sVWibbUgQCf6ChQ==, tableContent=null), ArticleFig(id=1177619526385545702, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153429499640271159, language=CN, label=图4, caption=
阴性基底粉加标(LNnT)色谱图, figureFileSmall=Fe5H1rH9RUoy7n9coXHWlQ==, figureFileBig=TLzCU3/sVWibbUgQCf6ChQ==, tableContent=null), ArticleFig(id=1177619526452654567, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153429499640271159, language=EN, label=Table 1, caption=
Conditions of gradient elution
, figureFileSmall=null, figureFileBig=null, tableContent=
| 时间/min | 流速/(mL/min) | 淋洗液/% | 曲线 |
| A | B |
| 0.0 | 0.5 | 92 | 8 | 线性 |
| 28.0 | 0.5 | 80 | 20 | 线性 |
| 29.0 | 0.5 | 80 | 20 | 线性 |
| 30.0 | 0.5 | 60 | 40 | 线性 |
| 34.5 | 0.5 | 60 | 40 | 线性 |
| 35.0 | 0.5 | 20 | 80 | 线性 |
| 39.5 | 0.5 | 20 | 80 | 线性 |
| 40.0 | 0.5 | 92 | 8 | 线性 |
| 48.0 | 0.5 | 92 | 8 | 线性 |
), ArticleFig(id=1177619526511374824, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153429499640271159, language=CN, label=表1, caption=
梯度洗脱条件
, figureFileSmall=null, figureFileBig=null, tableContent=
| 时间/min | 流速/(mL/min) | 淋洗液/% | 曲线 |
| A | B |
| 0.0 | 0.5 | 92 | 8 | 线性 |
| 28.0 | 0.5 | 80 | 20 | 线性 |
| 29.0 | 0.5 | 80 | 20 | 线性 |
| 30.0 | 0.5 | 60 | 40 | 线性 |
| 34.5 | 0.5 | 60 | 40 | 线性 |
| 35.0 | 0.5 | 20 | 80 | 线性 |
| 39.5 | 0.5 | 20 | 80 | 线性 |
| 40.0 | 0.5 | 92 | 8 | 线性 |
| 48.0 | 0.5 | 92 | 8 | 线性 |
), ArticleFig(id=1177619526591066601, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153429499640271159, language=EN, label=Table 2, caption=
Linear equations, correlation coefficients and MLODs and MLOQs of 4 kinds of human milk oligosaccharides
, figureFileSmall=null, figureFileBig=null, tableContent=
化合物
名称 | 线性方程 | 相关系数
(r2) | MLODs
/(mg/100 g) | MLOQs
/(mg/100 g) |
| 2'-FL | Y=2.3935X-5.9771 | 0.9999 | 1.84 | 6.12 |
| 3'-SL | Y=1.8276X-3.4217 | 0.9999 | 2.31 | 7.69 |
| 6'-SL | Y=1.8031X-3.4795 | 0.9999 | 1.87 | 6.25 |
| LNnT | Y=1.8218X-4.1695 | 0.9999 | 0.94 | 3.12 |
), ArticleFig(id=1177619526670758378, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153429499640271159, language=CN, label=表2, caption=
4种母乳低聚糖的线性方程、相关系数、MLODs和MLOQs
, figureFileSmall=null, figureFileBig=null, tableContent=
化合物
名称 | 线性方程 | 相关系数
(r2) | MLODs
/(mg/100 g) | MLOQs
/(mg/100 g) |
| 2'-FL | Y=2.3935X-5.9771 | 0.9999 | 1.84 | 6.12 |
| 3'-SL | Y=1.8276X-3.4217 | 0.9999 | 2.31 | 7.69 |
| 6'-SL | Y=1.8031X-3.4795 | 0.9999 | 1.87 | 6.25 |
| LNnT | Y=1.8218X-4.1695 | 0.9999 | 0.94 | 3.12 |
), ArticleFig(id=1177619526733672939, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153429499640271159, language=EN, label=Table 3, caption=
Recovery and precision test results of 4 kinds of human milk oligosaccharides
, figureFileSmall=null, figureFileBig=null, tableContent=
| 序号 | 简称 | 添加水平
/(mg/100 g) | 回收率
/% | RSDs
/% |
| 1 | 2'-FL | 10、700、2700 | 98.0、97.7、101.5 | 1.77、0.63、0.58 |
| 2 | 3'-SL | 10、100、2700 | 97.7、100.9、100.1 | 0.53、3.09、1.10 |
| 3 | 6'-SL | 10、70、2700 | 100.0、101.3、100.4 | 1.00、1.38、1.37 |
| 4 | LNnT | 10、70、2700 | 98.0、99.3、100.5 | 1.02、2.91、1.84 |
), ArticleFig(id=1177619526804976108, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153429499640271159, language=CN, label=表3, caption=
4种母乳低聚糖的回收率和精密度测试结果
, figureFileSmall=null, figureFileBig=null, tableContent=
| 序号 | 简称 | 添加水平
/(mg/100 g) | 回收率
/% | RSDs
/% |
| 1 | 2'-FL | 10、700、2700 | 98.0、97.7、101.5 | 1.77、0.63、0.58 |
| 2 | 3'-SL | 10、100、2700 | 97.7、100.9、100.1 | 0.53、3.09、1.10 |
| 3 | 6'-SL | 10、70、2700 | 100.0、101.3、100.4 | 1.00、1.38、1.37 |
| 4 | LNnT | 10、70、2700 | 98.0、99.3、100.5 | 1.02、2.91、1.84 |
), ArticleFig(id=1177619526859502061, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153429499640271159, language=EN, label=Table 4, caption=
Comparison between the results of this method and other methods
, figureFileSmall=null, figureFileBig=null, tableContent=
| 样品 | 检测方法 | 2'-FL/(mg/100 g) | t值 | 3'-SL/(mg/100 g) | t值 | 6'-SL/(mg/100 g) | t值 | LNnT/(mg/100 g) | t值 | t0.05,10 |
| A | 本方法 | 458 | 1.246 | 52 | 1.414 | 18 | 1.000 | 126 | 1.928 | 2.228 |
| T/SAFC 002—2024 | 460 | 52 | 19 | 128 |
| 标示值: 450 | 无标示值 | 无标示值 | 标示值: 120 |
| B | 本方法 | 15 | 1.472 | 16 | 1.249 | 71 | 1.917 | 377 | 1.917 |
| T/SAFC 002—2024 | 16 | 17 | 72 | 379 |
| 无标示值 | 无标示值 | 无标示值 | 标示值: 370 |
| C | 本方法 | 11 | 2.080 | 14 | 1.000 | 20 | 1.746 | 8 | 0.808 |
| T/SAFC 002—2024 | 12 | 15 | 21 | 8 |
| 无标示值 | 无标示值 | 无标示值 | 无标示值 | |
), ArticleFig(id=1177619526930805230, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153429499640271159, language=CN, label=表4, caption=
本方法与其他方法测定结果的比较
, figureFileSmall=null, figureFileBig=null, tableContent=
| 样品 | 检测方法 | 2'-FL/(mg/100 g) | t值 | 3'-SL/(mg/100 g) | t值 | 6'-SL/(mg/100 g) | t值 | LNnT/(mg/100 g) | t值 | t0.05,10 |
| A | 本方法 | 458 | 1.246 | 52 | 1.414 | 18 | 1.000 | 126 | 1.928 | 2.228 |
| T/SAFC 002—2024 | 460 | 52 | 19 | 128 |
| 标示值: 450 | 无标示值 | 无标示值 | 标示值: 120 |
| B | 本方法 | 15 | 1.472 | 16 | 1.249 | 71 | 1.917 | 377 | 1.917 |
| T/SAFC 002—2024 | 16 | 17 | 72 | 379 |
| 无标示值 | 无标示值 | 无标示值 | 标示值: 370 |
| C | 本方法 | 11 | 2.080 | 14 | 1.000 | 20 | 1.746 | 8 | 0.808 |
| T/SAFC 002—2024 | 12 | 15 | 21 | 8 |
| 无标示值 | 无标示值 | 无标示值 | 无标示值 | |
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