超高效液相色谱-三重四极杆质谱法检测油脂和油炸食品中7种杂环胺类物质

Determination of seven heterocyclic aromatic amines in oils and fried foods by ultra performance liquid chromatography-triple quadrupole mass spectrometry

建立了检测油脂及油炸食品中7种杂环胺类物质的超高效液相色谱-三重四极杆质谱(UPLC-MS/MS)的检测方法。以含1%(体积分数)氨水的乙腈溶液为提取液,采用乙腈饱和的正己烷脱脂,以PCX固相萃取柱为净化柱,10 mmol/L甲酸铵溶液(pH 6.8)和乙腈为流动相,采用Waters ACQUITY UPLC BEH C18反相色谱柱(50 mm×2.1 mm,1.7μm)梯度洗脱,流速为0.3 mL/min,在正离子扫描、多反应监测模式下测定,内标法定量。结果表明,杂环胺类物质在各自范围内,线性关系良好,相关系数大于0.999;在3个加标水平下,杂环胺类物质在油脂和油炸食品中的平均回收率为64.31%~113.8%,相对标准偏差为0.18%~9.26%,检出限(S/N=3)和定量限(S/N=10)分别为0.01~0.14 ng/g和0.09~0.38 ng/g。该方法具有灵敏、准确等优点,适用于油脂和油炸食品中杂环胺的确证检测。

An ultra performance liquid chromatography-triple quadrupole mass spectrometry(UPLC-MS/MS)method was developed for the determination of seven heterocyclic aromatic amines(HCAs)in oil and fried food samples.The samples were extracted with acetonitrile containing 1%(v/v)ammonia water,defatted by n-hexane saturated with acetonitrile,and cleaned up with PCX solid phase extraction column.The extracts were separated on a Waters ACQUITY UPLC BEH C18 reversed-phase column(50 mm×2.1 mm,1.7μm)with gradient elution by using acetonitrile-10 mmol/L ammonium formate aqueous solution as the mobile phase.Quantitative detection was performed by using a positive-ion electrospray ionization source in the multiple reaction monitoring(MRM)mode,employing an internal isotope standard.The method showed good linear relationships in the range of 0.5-100μg/L for the seven HCAs with correlation coefficients(R^2)>0.999.The average recoveries ranged from 64.31%to 113.8%with the relative standard deviations of 0.18%-9.26%at the three spiked levels in oil and fried food samples.The limits of detection(LODs)and limits of quantification(LOQs)were 0.01-0.14 ng/g and 0.09-0.38 ng/g,respectively.The method is sensitive,accurate,and suitable for the determination and confirmation of the seven HCAs in oil and fried food samples.