| With the rapid development of the functional food industry, functional food(health food) daily consumption is increasing, affecting food contact packaging materials in the migration of hazardous substances on the human body has been attached to quality-oriented education. Recent study shows that, in the functional food manufacturing process, the inevitable contact packaging materials used in the migration of bisphenol substances to foods, serious harm to human health, especially the impact of genetic brain development and immune function in infants. Bisphenol substances of this topic have 14 kinds: Bisphenol A(BPA), Bisphenol F(BPF), Tetrachlorobisphenol A(TCBPA), Tetrabromobisphenol A(TBBPA), Bisphenol A diglycidyl ether(BADGE), Bisphenol A diglycidyl ether(BADGE), Bisphenol A(2,3-dihydroxypropyl) glycidyl ether(BADGE-H2O), Bisphenol A(3-chloro-2-hydroxypropyl) glycidyl ether(BADGE-HCl), Bisphenol A bis(2,3-dihydroxypropyl) ether(BADGE-2H2O), Bisphenol A bis(3-chloro-2-hydroxypropyl) ether(BADGE-2HCl), Bisphenol A(3-chloro-2-hydroxy propyl)(2,3-dihydroxypropyl) ether(BADGE-HCl-H2O), Bisphenol F diglycidyl ether(BFDGE), Bisphenol F bis(2,3-dihydroxypropyl) ether(BFDGE-2H2O), Bisphenol F bis(3-chloro-2-hydroxypropyl) ether(BFDGE-2HCl), Bisphenol S(BPS).Contact packaging materials inevitably use of bisphenol substances in functional food storage and other processing and transportation process will migrate to the food, V the serious consequences of serious harm to human health, teratogenic, carcinogenic, mutagenic, etc., especially the impact of infant brain development and immune genetic function. The scientific reports home and abroad detected only some of them, 11 is the most, which is far away from overall coverage.This topic mainly focus on the detection methods of bisphenol substances residues in functional food. For sample preparation, study is deep on optimization of sample extraction and purification steps; For detection method, take the "5 mmol/L ammonium acetate solution(containing 1‰ formic acid)-acetonitrile" as the mobile phase to gradient elution and take the Thermo Aquasil C18(150 mm×4.6 mm,3.0 μm) column and Waters Atlantis T3(150 mm × 2.1 mm,3.0 μm) column to separate the analytes, and meanwhile take HPLC-MS/MS for qualitative and quantitative study.A high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) method with Qu ECh ERS was developed for the determination of 4 bisphenol substances residues in functional food, including BPA, BPF, TCBPA and TBBPA. Quantified by matrix-matched external standard method, the calibration curves showed good linearity in 0.5~50.0 μg/kg range with correlation coefficients greater than 0.9990. The limits of quantitation(LOQs, S/N>10) were in the range of 0.9~1.5 μg/kg and the limits of detection(LODs, S/N>3) were 0.2~0.4 μg/kg. The recoveries of the 4 bisphenol substances spiked at three levels(2.0 μg/kg, 5.0 μg/kg, 10.0 μg/kg) with different concentration ranged from 81.5% ~ 101.2%, 83.0% ~ 102.0% and 73.3%~88.1% in milk powder, oral solution and oil capsule, with the RSDs ranged from 3.5%~9.3%, 3.5%~9.6% and 3.6%~9.5%.A high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) method with Qu ECh ERS was developed for the determination of 10 bisphenol substances residues in functional food, including BADGE, BADGE, BADGE-H2 O, BADGE-HCl, BADGE-2H2 O, BADGE-2HCl, BADGE-HCl-H2 O, BFDGE, BFDGE-2H2 O, BFDGE-2HCl and BPS. Quantified by matrix-matched external standard method, the calibration curves showed good linearity in 0.5~50.0 μg/kg range with correlation coefficients greater than 0.9990. The limits of quantitation(LOQs, S/N>10) were in the range of 0.4~1.7 μg/kg and the limits of detection(LODs, S/N>3) were 0.1~0.5 μg/kg. The recoveries of the 10 bisphenol substances spiked at three levels(2.0 μg/kg, 5.0 μg/kg, 10.0 μg/kg) with different concentration ranged from 79.3%~110.3%, 80.1%~106.5% and 70.5%~87.9% in milk powder, oral solution and oil capsule, with the RSDs ranged from 5.9%~10.5%, 6.0%~9.6% and 5.8%~10.4%.A high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) method with Qu ECh ERS was developed for the determination of 14 bisphenol substances residues in functional food, including BPA, BPF, TCBPA, TBBPA, BADGE, BADGE, BADGE-H2 O, BADGE-HCl, BADGE-2H2 O, BADGE-2HCl, BADGE-HCl-H2 O, BFDGE, BFDGE-2H2 O, BFDGE-2HCl and BPS. The quantification was carried out by matrix-matched calibration curve and used internal standard(BPA-d16, TBBPA-d10 and BPS-c13). The calibration curves showed good linearity in each range with correlation coefficients greater than 0.9990(TBBPA:2.5~250 μg/kg,BADGE-2HCl:1.0~100.0 μg/kg,others:0.5~50 μg/kg). The recoveries of the 14 bisphenol substances spiked at three levels with different concentration ranged from 89.2%~107.1%, 89.3%~105.3% and 84.0%~95.8% in infant milk powder, infant nutritious cereal and infant supplement puree, with the RSDs ranged from 5.6%~9.3%, 5.0%~9.4% and 5.9%~9.2%(TBBPA:25~125 μg/kg,BADGE-2HCl:10.0~50.0 μg/kg,others:5~25 μg/kg). The limits of quantitation(LOQs, S/N>10) were in the range of 1.0~2.0 μg/kg and the limits of detection(LODs, S/N>3) were 0.3~0.7 μg/kg.This study has established three kinds of detection method to analysis bisphenol substances by matrix-matched external standard or internal standard method in functional food. As to the amount of bisphenol substances, the established method for simultaneous determination is 14 bisphenol substances, more than 11 bisphenol substances in literature reported. Compared with 2.0-10.0 mg/kg of LOQs in literature reported, 14 bisphenol substances are much more better, ranged from 0.9 to 1.5 μg/kg. Meanwile, the dedication method established in this study are celebrated for time-saving, sensitivity, accuracy and precision, which also meet the residual analysis standard and has already been successfully applied to practice. |
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