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 based on high performance liquid chromatography-tandem mass spectrom-etry(HPLC-MS / MS)for the simultaneous determination of 12 bisphenol substances in function-al foods(powder,tablet,capsule)was presented. The samples were extracted by acetonitrile containing 1%(v / v)acetic acid followed by further cleaned up using matrix solid-phase disper-sion to remove matrix interferences. The separation of the 12 bisphenol substances was per-formed on a Thermo Aquasil C 18 column(150 mm×4. 6 mm,3. 0 μm),and determined in the positive and negative MRM modes by MS / MS using matrix-matched external standard method. The results demonstrated that the calibration curves were of good linearity with the correlation coefficients greater than 0. 99. The limits of detection(LODs,S / N>3)were in the range of 0. 1-0. 5 μg / kg and the limits of quantitation(LOQs,S / N>10)were 0. 4-1. 7 μg / kg. The recover-ies of the 12 bisphenol substances spiked at three levels(2. 0,5. 0 and 10. 0 μg / kg)in matrix ranged from 60. 5% to 116. 3% with the relative standard deviations(RSDs)of 6. 8% to 11. 2% . The established method is simple,time-saving and sensitive. It can meet the requirements for current regulations while achieving qualitative and quantitative determination of the 12 bisphenol substances in functional foods.
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