采用一步式净化的新型净化方式,基于气相色谱-四极杆-飞行时间质谱(gas chromatography-quadrupole-time of flight-mass spectrometry,GC-Q-TOF-MS)技术建立肉制品中包括己二酸酯、柠檬酸酯、有机磷酸酯、癸二酸酯和苯甲酸酯等不同家族的46种替代型增塑剂(alternative plasticizers,APs)的高通量、快速筛选技术与定量分析方法.样品经乙腈提取,SinChERS-General柱一步式净化,GC-Q-TOF-MS全扫描模式采集质谱信息,利用自建的46种APs高分辨质谱数据库对目标物进行快速筛查和定量分析.为提高筛查结果的准确性,考察不同提取溶剂的提取效率和不同类型净化剂的除杂能力,对GC分离条件和高分辨质谱筛查参数进行优化,从线性范围、准确度等方面对定量方法进行考察.结果表明:在0.01～0.2 mg/L范围内,46种APs呈现较好的线性关系(R2＞0.99),筛查限为0.03～0.05 mg/kg,定量限为0.05～0.1 mg/kg,在0.1、0.2、0.5 mg/kg加标水平下,平均加标回收率为68.6％～119.3％,相对标准偏差为0.6％～8.9％.将该筛查策略应用于100批实际样品检测,1批猪头肉检出己二酸二(2-乙基己基)酯、3批火腿肠检出乙酰柠檬酸三丁酯.综上,该方法通过一次净化与检测可实现回顾性分析,有效缩短检测时间、降低经济成本、提高检测效率,实现肉制品中46种APs的高通量快速筛查和定量分析,可为肉制品中APs污染监测和风险预警工作提供技术支持.
High Throughput Screening of 46 Alternative Plasticizers in Meat Products by Single-Step Quick,Easy,Cheap,Effective,Rugged and Safe(Sin-QuEChERS)Purification Coupled with Gas Chromatography-Quadrupole-Time of Flight-Mass Spectrometry(GC-Q-TOF-MS)
A high throughput rapid screening and quantitative analysis method based on a new purification method of single-step purification combined with gas chromatography-quadrupole-time of flight-mass spectrometry(GC-Q-TOF-MS)was developed for 46 alternative plasticizers(APs)in meat products,including adipate,citrate,organophosphatate,sebacate and benzoate.Samples were extracted with acetonitrile and purified through a SinChERS-General column,mass spectrometric information was collected in the full scan mode,and a high-resolution MS library of the 46 APs was created for rapid screening and quantitative determination of the target analytes.In order to improve the accuracy of the screening results,the extraction efficiency of different extraction solvents and the impurity removal ability of different purifying agents were investigated.The GC separation conditions and the high-resolution MS screening parameters were optimized,and the quantitative method was validated from the aspects of linear range and accuracy.The calibration curves for the 46 APs showed a good linear relationship(R2＞0.99)in the range of 0.01-0.2 mg/L,the screening detection limit was 0.03-0.05 mg/kg,and the limit of quantitation was 0.05-0.1 mg/kg.The average spiked recoveries were 68.6％-119.3％and the relative standard deviations(n=6)were 0.6％-8.9％at three different spiked levels(0.1,0.2,0.5 mg/kg).The screening strategy was applied to 100 batches of actual samples.Di(2-ethylhexyl)adipate was detected in one batch of porcine head meat,and acetyl tributyl citrate in three batches of sausages.The proposed method is characterized by short detection time,low cost and high detection efficiency and allows rapid screening and quantitative analysis of the 46 APs in meat products,which provides technical support for the monitoring and risk early warning of APs contamination in meat products.
gas chromatography-quadrupole-time of flight-mass spectrometryalternative plasticizershigh throughput screeningmeat products
万方数据
维普
