食品安全质量检测学报
食品安全質量檢測學報
식품안전질량검측학보
FOOD SAFETY AND QUALITY DETECTION TECHNOLOGY
2015年
4期
1504-1510
,共7页
李洪燕%李秀英%陈俊禧%刘冬虹%林森煜%卢宇靖%黄金凤
李洪燕%李秀英%陳俊禧%劉鼕虹%林森煜%盧宇靖%黃金鳳
리홍연%리수영%진준희%류동홍%림삼욱%로우정%황금봉
泛酸%超高压液相色谱-串联质谱法%同位素稀释%维生素营养液
汎痠%超高壓液相色譜-串聯質譜法%同位素稀釋%維生素營養液
범산%초고압액상색보-천련질보법%동위소희석%유생소영양액
pantothenic acid%ultra high performance liquid chromatography-tandem mass spectrometry%isotope dilution%multivitamin supplement solution
目的:建立测定维生素营养液中泛酸含量的同位素稀释-超高压液相色谱-串联质谱法(ID-UHPLC- MS/MS)。方法样品经高氯酸水溶液涡旋提取和除杂、超纯水稀释后,以HSS T3色谱柱和0.1%(v:v)甲酸水溶液-乙腈进行梯度洗脱分离,以串联质谱的多反应监测模式检测,内标法定量。结果泛酸在5~1000μg/L范围内具有良好的线性关系,相关系数(R2)为0.9998;方法检出限为0.02 mg/100 g,定量限为0.07 mg/100 g,3个添加水平的回收率为93.4%~105%,相对标准偏差(n=6)为2.3%~4.4%,日间相对标准偏差(n=3)为2.72%。结论本方法操作简便、分析速度快、灵敏度高、重复性好,为维生素营养液中泛酸含量的定性定量分析提供了可靠的依据。
目的:建立測定維生素營養液中汎痠含量的同位素稀釋-超高壓液相色譜-串聯質譜法(ID-UHPLC- MS/MS)。方法樣品經高氯痠水溶液渦鏇提取和除雜、超純水稀釋後,以HSS T3色譜柱和0.1%(v:v)甲痠水溶液-乙腈進行梯度洗脫分離,以串聯質譜的多反應鑑測模式檢測,內標法定量。結果汎痠在5~1000μg/L範圍內具有良好的線性關繫,相關繫數(R2)為0.9998;方法檢齣限為0.02 mg/100 g,定量限為0.07 mg/100 g,3箇添加水平的迴收率為93.4%~105%,相對標準偏差(n=6)為2.3%~4.4%,日間相對標準偏差(n=3)為2.72%。結論本方法操作簡便、分析速度快、靈敏度高、重複性好,為維生素營養液中汎痠含量的定性定量分析提供瞭可靠的依據。
목적:건립측정유생소영양액중범산함량적동위소희석-초고압액상색보-천련질보법(ID-UHPLC- MS/MS)。방법양품경고록산수용액와선제취화제잡、초순수희석후,이HSS T3색보주화0.1%(v:v)갑산수용액-을정진행제도세탈분리,이천련질보적다반응감측모식검측,내표법정량。결과범산재5~1000μg/L범위내구유량호적선성관계,상관계수(R2)위0.9998;방법검출한위0.02 mg/100 g,정량한위0.07 mg/100 g,3개첨가수평적회수솔위93.4%~105%,상대표준편차(n=6)위2.3%~4.4%,일간상대표준편차(n=3)위2.72%。결론본방법조작간편、분석속도쾌、령민도고、중복성호,위유생소영양액중범산함량적정성정량분석제공료가고적의거。
Objective To develop a simple and rapid method for determination of pantothenic acid in multivitamin supplement by ultra high performance liquid chromatography - tandem mass spectrometry with isotope dilution (ID-UHPLC-MS/MS).Methods The sample was extracted and purified by perchloric acid solution, and separated on an HSS T3 UPLC column with acetonitrile and 0.1% formic acid solution as mobile phase under gradient elution mode, then detected with tandem mass spectrometry under ESI at positive and multiple reaction monitoring (MRM) mode. Stable isotope was used as an internal standard for quantification. Results Pantothenic acid has a good linear relationship in the range of 5~1000μg/L, the limit of detection (LOD) and quantitation (LOQ) of the method was 0.02 mg/100 g and 0.07 mg/100 g respectively. The fine recovery (93.4%~105%), the relative standard deviation (2.3%~4.4%,n=6) and inter-day with RSD (2.72%, n=3) of this method were also obtained.Conclusion The proposed method was successfully applied to determine pantothenic acid in multivitamin supplement. Compared with the standard method, the proposed method was sensitive, rapid, and accurate. It provides a rapid approach for the analysis of pantothenic acid in complex matrix multivitamin supplement solution.