化学分析计量
化學分析計量
화학분석계량
CHEMICAL ANALYSIS AND METERAGE
2015年
1期
1-4
,共4页
陈晖%方华%张怡评%陈伟珠%洪专%易瑞灶
陳暉%方華%張怡評%陳偉珠%洪專%易瑞竈
진휘%방화%장이평%진위주%홍전%역서조
海藻糖%标准样品%离子色谱法%定值%不确定度
海藻糖%標準樣品%離子色譜法%定值%不確定度
해조당%표준양품%리자색보법%정치%불학정도
trehalose%certified reference material%ion chromatography%certification%uncertainty
研制了海藻糖国家标准样品。以食品级海藻糖粗品为原料,纯化制备海藻糖,采用红外光谱(IR)、质谱和核磁共振谱(NMR)以及单晶衍射等方法进行结构确证。样品分装成400瓶后,采用离子色谱法进行均匀性、稳定性检验和定值分析。从样品中随机抽取15瓶进行均匀性检验,经F检验表明,在95%的置信区间范围内,样品均匀性良好。在40℃下,经过24个月稳定性考察,结果表明样品稳定性良好。标准样品经国内8家具有分析资质的实验室进行协同定值,并评定了定值结果的不确定度,海藻糖标准样品定值结果为99.72%,扩展不确定度为0.26%(k=1.96)。该标准样品达到国家标准样品的技术要求,可用于有关海藻糖的方法校正和质量控制。
研製瞭海藻糖國傢標準樣品。以食品級海藻糖粗品為原料,純化製備海藻糖,採用紅外光譜(IR)、質譜和覈磁共振譜(NMR)以及單晶衍射等方法進行結構確證。樣品分裝成400瓶後,採用離子色譜法進行均勻性、穩定性檢驗和定值分析。從樣品中隨機抽取15瓶進行均勻性檢驗,經F檢驗錶明,在95%的置信區間範圍內,樣品均勻性良好。在40℃下,經過24箇月穩定性攷察,結果錶明樣品穩定性良好。標準樣品經國內8傢具有分析資質的實驗室進行協同定值,併評定瞭定值結果的不確定度,海藻糖標準樣品定值結果為99.72%,擴展不確定度為0.26%(k=1.96)。該標準樣品達到國傢標準樣品的技術要求,可用于有關海藻糖的方法校正和質量控製。
연제료해조당국가표준양품。이식품급해조당조품위원료,순화제비해조당,채용홍외광보(IR)、질보화핵자공진보(NMR)이급단정연사등방법진행결구학증。양품분장성400병후,채용리자색보법진행균균성、은정성검험화정치분석。종양품중수궤추취15병진행균균성검험,경F검험표명,재95%적치신구간범위내,양품균균성량호。재40℃하,경과24개월은정성고찰,결과표명양품은정성량호。표준양품경국내8가구유분석자질적실험실진행협동정치,병평정료정치결과적불학정도,해조당표준양품정치결과위99.72%,확전불학정도위0.26%(k=1.96)。해표준양품체도국가표준양품적기술요구,가용우유관해조당적방법교정화질량공제。
Trehalose certified reference material was developed.Trehalose was purified from the crude product. The structure of trehalose certified reference material was comfirmed by infrared spectroscopy (IR),mass spectrometry, NRM and XRD.Trehalose was divided into 400 bottles.The homogeneity and stability testing and quantitative analysis were evaluated by ion chromatography method.According to analysis procedure of homogeneity,15 bottles of sample were randomly taken from 400 bottles,and the results were validated by F-test statistical methods.The stability inspec-tion was carried on the long-term(24 months),and the results indicated that the period for trehalose storage was 24 months at 40℃.A cooperative certification was conducted by 8 qualified laboratories.The certified purity value of the reference material of trehalose was 99.72%with relative expaned uncertainty of 0.26%(k=1.96).The reference material can conform to the technical requirement of the certified reference material,and it can be used for validation and quality control regarding trehalose.