摘要
利用色谱保留时间、紫外吸收光谱及质谱对首次从小麦中发现的富马酸成分进行了确证,并建立了小麦中富马酸含量的超高效液相-串联质谱检测法和高效液相色谱-二极管阵列检测法。样品采用1%氨水-乙腈(体积比为1:1)提取,稀释后进样测定,超高效液相-串联质谱法采用亲水的HILIC色谱柱(50mm×2.1mm,1.7μm)分离,以乙腈-10mmol/L甲酸铵(体积比为85:15)为流动相,电喷雾负离子检测,多反应检测模式定性和定量;高效液相色谱-二极管阵列检测法采用传统的反相C18色谱柱(4.6mm×250mm,5μm)分离,以50mmol/L磷酸二氢铵(pH2.4)为流动相,在波长210nm处检测。小麦样品中的目标物与富马酸标准品具有相同的色谱保留时间、紫外吸收光谱和质谱,确定该目标物为富马酸,而且不同产地的4批小麦样品均检出富马酸;含量测定时的提取方法回收率及重现性良好,2种检测方法均不存在干扰,线性关系良好。首次从小麦中发现并确证了富马酸成分,建立的2种含量检测方法均能满足检测要求。
Chromatographic retention time, UV absorption spectrum and mass spectrometry were used to confirm a new composition as fumaric acid found in wheat, and two quantitative analysis methods of fumaric acid in wheat have been developed. An ultra performance liquid chromatograph-tandem mass spectrometry（UPLC-MS/MS） instrument and a high performance liquid chromatograph-diode array detector（HPLC-DAD） instrument were used for the determination. Sample preparation involves extraction with 1% ammonia-water solution/acetonitrile（1：1, v/v）, and dilution with right solution before detection. UPLC-MS/MS separation was performed on a HILIC（50 mm×2.1 mm, 1.7 μm） column eluted with acetonitrile/10 mmol/L ammonium formate（85：15, v/v）, qualitative and quantitative analysis were achieved by electrospray ionization（ESI） negative ion mode with multiple reaction monitoring（MRM）. HPLC was performed on a traditional C18（4.6 mm×250 mm, 5 μm） column with DAD detection at 210 nm using 50 mmol/L ammonium dihydroyen phosphate solution（pH2.4） as mobile phase. The results show that the targets in wheat have the same chromatographic retention time, UV absorption spectrum and mass spectrometry as fumaric acid standard, so the taget was confirmed as fumaric acid. And fumaric acid were detected in four wheat samples from different area. The quantitative analysis methods showed good recovery and reproducibility. Fumaric acid in measured samples was separated completely. The calibration curve showed good linear relationship. A new composition as fumaric acid was first found an confirmed in wheat, and the two quantitative analysis methods were suitable for determination of fumaric acid.
出处
《食品科技》
CAS
北大核心
2011年第9期318-321,326,共5页
Food Science and Technology
基金
陕西省农业科技攻关项目(2010K01-19-4)
国家质检总局科研项目(2009IK285)
关键词
小麦
富马酸
发现
确证
含量
超高效液相色谱-串联质谱
高效液相色谱
wheat
fumaric acid
discovery
confirmation
quantitative analysis
ultra performance liquid chromatography-tandem mass spectrometry
high performance liquid chromatography
