分析化学
分析化學
분석화학
CHINESE JOURNAL OF ANALYTICAL CHEMISTRY
2009年
12期
1765-1770
,共6页
盛旋%胡艳云%张蕾%孙昊%郑屏%陶发荣%杨嫣嫣%杭吉
盛鏇%鬍豔雲%張蕾%孫昊%鄭屏%陶髮榮%楊嫣嫣%杭吉
성선%호염운%장뢰%손호%정병%도발영%양언언%항길
石蜡%蒸发光散射%液相色谱%食品
石蠟%蒸髮光散射%液相色譜%食品
석사%증발광산사%액상색보%식품
Paraffin wax%evaporative light-scattering%liquid chromatography%food
采用液相色谱(HPLC)结合蒸发光散射检测器(ELSD)对食品中的石蜡残留物进行了分析和检测.利用正相色谱柱对石蜡和非石蜡组分进行了分离,而无需对石蜡组分进行逐一分离.利用t检验,对构成石蜡的烷烃组分在ELSD检测器上的线性响应进行了显著性误差分析,结果显示,石蜡中烷烃组分具有相似的线性响应.以此为定量依据,实现了食品中石蜡含量的快速定量分析.并对HPLC-ELSD的检测和确证结果与GC-MS法进行了对比.方法的线性范围为10~500 mg/L,相关系数为0.9988;检出限为1 mg/L.以10, 50和100 mg/kg浓度水平添加石蜡时,其回收率在84.6%~105.4%之间,相对标准偏差为5.4%~7.2%.
採用液相色譜(HPLC)結閤蒸髮光散射檢測器(ELSD)對食品中的石蠟殘留物進行瞭分析和檢測.利用正相色譜柱對石蠟和非石蠟組分進行瞭分離,而無需對石蠟組分進行逐一分離.利用t檢驗,對構成石蠟的烷烴組分在ELSD檢測器上的線性響應進行瞭顯著性誤差分析,結果顯示,石蠟中烷烴組分具有相似的線性響應.以此為定量依據,實現瞭食品中石蠟含量的快速定量分析.併對HPLC-ELSD的檢測和確證結果與GC-MS法進行瞭對比.方法的線性範圍為10~500 mg/L,相關繫數為0.9988;檢齣限為1 mg/L.以10, 50和100 mg/kg濃度水平添加石蠟時,其迴收率在84.6%~105.4%之間,相對標準偏差為5.4%~7.2%.
채용액상색보(HPLC)결합증발광산사검측기(ELSD)대식품중적석사잔류물진행료분석화검측.이용정상색보주대석사화비석사조분진행료분리,이무수대석사조분진행축일분리.이용t검험,대구성석사적완경조분재ELSD검측기상적선성향응진행료현저성오차분석,결과현시,석사중완경조분구유상사적선성향응.이차위정량의거,실현료식품중석사함량적쾌속정량분석.병대HPLC-ELSD적검측화학증결과여GC-MS법진행료대비.방법적선성범위위10~500 mg/L,상관계수위0.9988;검출한위1 mg/L.이10, 50화100 mg/kg농도수평첨가석사시,기회수솔재84.6%~105.4%지간,상대표준편차위5.4%~7.2%.
A method was proposed for the separation and determination of paraffin waxes in food by HPLC-evaporative light scattering detection (ELSD). A normal-phase column was used to separate nonparaffinic and paraffinic materials without resolving the latter into individual components. The t-test method was adopted for the evaluation of mean difference between response factors of n-alkanes in paraffin waxes on ELSD detector. No mean difference was obtained between response factors, which can be used for quantitative determination of paraffin waxes in food. The determination results obtained by HPLC-ELSD were compared with those by GC-MS. The linear range for the determination of paraffin waxes was in the range from 10 to 500 mg/L with a correlation coefficient of 0.9988, and the limit of detection was 1.0 mg/L. With the spiking level of 10, 50 and 100 mg/kg, the recovery ranged from 84.6% to 105.4% and the relative standard deviation ranging from 5.4% to 7.2%. The proposed method is simple, fast and sensitive.