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建立了采用高效液相色谱-串联质谱(HPLC-MS/MS)同时测定粉剂、片剂和胶囊剂等保健食品中12种双酚类化合物的检测方法。样品中双酚类化合物经1%(v/v)乙酸乙腈溶液提取,QuEChERS方法净化;12种化合物经Thermo Aquasil C18色谱柱(150 mm×4.6 mm,3.0μm)分离后,分别在串联质谱正、负离子多反应监测(MRM)模式下检测,基质匹配外标法定量。研究结果表明,在0.5~50.0μg/kg内,12种双酚类化合物的线性相关系数均大于0.99,方法的检出限(S/N>3)为0.1~0.5μg/kg,定量限(S/N>10)为0.4~1.7μg/kg,不同基质的保健食品在3个添加水平(2.0、5.0和10.0μg/kg)下的回收率为60.5%~116.3%(n=6),相对标准偏差(RSD)为6.8%~11.2%(n=6)。方法操作简单、耗时短、灵敏度高,满足现行法规要求,可实现保健食品中双酚类化合物的定性和定量测定。
A method for the simultaneous determination of 12 bisphenols in health food such as powder, tablet and capsule by HPLC-MS / MS was established. The samples were extracted with 1% (v / v) acetic acid in acetonitrile and purified by QuEChERS method. Twelve compounds were separated on a Thermo Aquasil C18 column (150 mm × 4.6 mm, 3.0 μm) , Negative ion multiple reaction monitoring (MRM) mode detection, matrix matching external standard method. The results showed that the linear correlation coefficients of 12 bisphenols were all greater than 0.99 in the range of 0.5-50.0 μg / kg, and the detection limit (S / N> 3) was 0.1-0.5 μg / kg. The limit of quantification S / N> 10) was 0.4-1.7 μg / kg. The recoveries of health food supplemented with different matrices were 60.5% -116.3% (n = 6) at the three supplementation levels (2.0, 5.0 and 10.0 μg / kg) The relative standard deviations (RSDs) ranged from 6.8% to 11.2% (n = 6). The method has the advantages of simple operation, short time-consuming and high sensitivity, meeting the requirements of the current laws and regulations and enabling the qualitative and quantitative determination of bisphenols in health food.