超高效液相色谱-串联质谱法检测花生中18 种塑化剂

Determination of 18 kinds of plasticizers in peanuts by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高效液相色谱-串联质谱法  花生  通量高  塑化剂  风险评估

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  peanuts  high throughput  plasticizers  risk assessment

中文摘要:

      目的 建立超高效液相色谱-串联质谱法检测花生中18种塑化剂。方法 样品经乙腈超声提取并低温低速离心后, 直接取上清液于–18℃冰箱中冷冻至少2 h, 上清液经0.22 μm滤膜过滤后通过Shim-pack XR-ODSШ反相色谱柱(2.0 mm×150 mm, 2.2 μm)进行分离, 最后经三重四极杆质谱在多反应监测模式下用外标法定量测定。结果 在最佳分析条件下, 各塑化剂靶标线性范围均良好, 相关系数(r2)均大于0.999; 检出限和定量限分别在0.0004~1.0000 μg/kg和0.0012~3.0000 μg/kg范围内; 在3个不同浓度下的加标回收率位于75.26%~114.54%之间, 相对标准偏差为1.08%~8.00% (n=6)。结论 该方法操作简单、稳定可靠、检测通量高、检测成本低, 有望用于大批量花生样品中塑化剂质量安全风险评估筛查及验证分析, 以期为政府部门大宗粮油质量安全监管提供技术支撑。

英文摘要:

      Objective To establish a method for the determination of 18 kinds of plasticizers in peanuts by ultra performance liquid chromatography-tandem mass spectrometry. Methods After ultrasonic extraction with acetonitrile and centrifugation at low temperature and speed, the supernatants were collected and refrigerated in a –18℃ for at least 2 h. Following filted through 0.22 μm filter membrane, the supernatants were separated by Shim-pack XR-ODS reverse phase chromatography column (2.0 mm×150 mm, 2.2 μm) and quantitatively determined by triple quadrupole mass spectrometry in multiple reaction monitoring mode using external standard method. Results Under the optimal analysis conditions, the linear range of each plasticizer target was good, and the correlation coefficient (r2) was>0.999. The limits of detection and quantification were within the ranges of 0.0004–1.0000 μg/kg and 0.0012–3.0000 μg/kg, respectively. The recoveries at 3 different concentrations ranged from 75.26% to 114.54%, and the relative standard deviations ranged from 1.08% to 8.00% (n=6). Conclusion This method is simple, stable and reliable, has high detection throughput and low detection cost, and is expected to be used for quality and safety risk assessment, screening and verification analysis of plasticizers in large quantities of peanuts samples, in order to provide technical support for quality and safety supervision of bulk grain and oil by government departments.