超高效液相色谱-串联质谱法快速检测预制调理羊肉串中15种杂环胺

Rapid determination of 15 kinds of heterocyclic amines in prefabricated mutton kebabs by ultra performance liquid chromatogram-tandem mass spectrometry

中文关键词:  预制调理羊肉串  杂环胺  超高效液相色谱-串联质谱法(UPLC-MS/MS)  QuEChERS法

英文关键词:prefabricated mutton kebabs  heterocyclic amines  ultra performance liquid chromatography-tandem mass spectrometry  QuEChERS method

中文摘要:

      目的 基于超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectroscopy, UPLC-MS/MS)建立预制调理烤制羊肉串样品中15种杂环胺(heterocyclic aromatic amines, HAAs)的高通量快速检测方法。方法 将预制调理羊肉串烤制后, 对固相萃取柱萃取法(Oasis PRiME HLB柱和Oasis MCX柱)、分散固相萃取法(QuEChERS)的净化效率进行评估; 得到净化物后经T3色谱柱(150 mm×2.1 mm, 1.8 μm)分离, 以乙腈和15 mmol/L甲酸铵溶液为流动相, 梯度洗脱分离, 采用串联三重四极杆质谱法对15种HAAs进行定量分析。结果 在一定检测范围内, 15种HAAs的线性良好, 相关系数(r2)在0.9979~0.9997之间, 检出限和定量限分别是0.002~0.017 ng/g和0.008~0.050 ng/g, 加标回收率为81.3%~113.2%, 相对标准偏差(relative standard deviations, RSDs)不大于11.9%。结论 该方法前处理效率高, 灵敏度高, 重现性好, 可用于预制调理烤制羊肉串样品中15种HAAs的快速检测, 为日后建立预制食品国家标准与法规提供方法依据。

英文摘要:

      Objective To establish a high throughput method for the rapid detection of 15 kinds of heterocyclic aromatic amines (HAAs) in preprepared mutton kebabs based on ultra performance liquid chromatogram-tandem mass spectrometry (UPLC-MS/MS). Methods After the preprepared mutton kebabs were grilled, the purification efficiency of solid phase extraction column extraction method (Oasis PRiMEHLB and MCX), dispersed solid phase extraction method (QuEChERS) was evaluated; the purified substance was separated by chromatographic column of T3 column (150 mm×2.1 mm, 1.8 μm) with gradient elution. Acetonitrile and 15 mmol/L ammonium formate solution were mobile phases. The 15 kinds of HAAs were detected and quantitatively analyzed by tandem triple quadrupole mass spectrometry. Results The method linearity was observed in a certain detection range for 15 kinds of HAAs, with determination coefficients (r2) between 0.9979 and 0.9997. Limits of detection and limits of quantification were in the ranges of 0.002?0.017 ng/g and 0.008?0.050 ng/g, respectively. The recoveries were 81.3%?113.2% and the relative standard deviations (RSDs) were no more than 11.9%. Conclusion This method has higher pretreatment efficiency, high sensitivity, and good reproducibility, which can be used for quickly quantitative determination of 15 kinds of HAAs in prefabricated mutton kebabs, which provides a method basis for the establishment of national standards and regulations for prepared food in the future.