摘要
目的建立一种同时测定熟肉制品中7种常用人工合成色素的固相萃取超快速液相色谱-串联质谱UFLC-MS/MS分析方法。方法熟肉制品用混合提取液提取后,用WAX固相萃取小柱净化,以乙腈和5 mmol/L乙酸铵水溶液为流动相,采用梯度洗脱方式在Shim-pack XR-ODS II色谱柱（75 mm×2.0 mm i.d.,2.2μm）上进行分离,以电喷雾负离子模式进行质谱分析。结果 7种人工合成色素在检测范围内均具有良好的线性关系（r〉0.999）,方法的定量限0.7-5.0μg/kg,熟肉制品的回收率88.2%-106.5%,RSDs 1.2%-5.0%。结论 UFLC-MS/MS法灵敏度高、重现性好、分析速度快,可用于熟肉制品中人工合成色素的确证检测。
Objective A method based on ultrafast liquid chromatography-tandem mass spectrometry（ UFLC-MS / MS） has been developed for the simultaneous determination of seven synthetic pigments in cooked meat product. Methods After the cooked meat products were extracted by mixed extraction agent, purified by WAX column,the UFLC separation was performed on a Shim-pack XR-ODS II column（ 75 mm× 2. 0 mm,2. 2 μm） with a linear gradient elution program of acetonitrile and ammonium acetate（ Am Ac,5 mmol / L） as the mobile phase. Electrospray ionization was applied and operated in the negative ion mode. Results The limits of quantitation（ LOQs） for the seven synthetic pigments were in the range of 0. 7- 5. 0 μg / kg. The calibration curves showed good linearities for the seven analytes in their detection ranges,and the correlative coefficients（ r） were more than 0. 999. The recoveries were between 88. 2%- 106. 5%with the RSDs in the range of 1. 2%- 5. 0%. Conclusion The method is sensitive,reproducible,quick and adapts to the simultaneous determination of the seven synthetic pigments in cooked meat product.
出处
《卫生研究》
CAS
CSCD
北大核心
2015年第4期636-640,共5页
Journal of Hygiene Research
基金
浙江省自然科学基金(No.LY13B050003)
宁波市自然科学基金(No.2013A610243)
浙江省医药卫生科学研究基金(No.2013KYA187)
关键词
超快速液相色谱-串联质谱法
固相萃取
熟肉制品
人工合成色素
ultrafast liquid chromatography-tandem mass spectrometry（UFLC-MS / MS）
solid phase extraction（SPE）
cooked meat product
synthetic
