同位素稀释-超高效液相色谱-三重四极杆串联质谱法同时测定蔬菜水果中双酚A和双酚S

Simultaneous determination of bispheol A and bisphenol S in vegetables and fruits by isotope dilution-ultra performance liquid chromatography-triple quadrupole tandem mass spectrometry

目的建立蔬菜、水果中双酚A(BPA)、双酚S(BPS)含量同时测定的同位素稀释-超高效液相色谱-三重四极杆串联质谱(UPLC-MS/MS)分析方法,测定河南省市售蔬菜、水果中BPA、BPS含量。方法试样加入BPA、BPS同位素内标,乙腈超声提取,GCB固相萃取柱净化,甲醇水梯度洗脱,ACQUITY UPLCTMBEH C18柱(100 mm×2.1 mm,1.7μm)分离,电喷雾离子源负离子扫描(ESI-)多反应监测(MRM)模式测定,空白基质匹配标准曲线、内标法定量。结果 BPA、BPS分别在0.5μg/L~20μg/L、0.05μg/L~2.0μg/L内线性关系良好,相关系数(r)均> 0.999,方法检出限(LOD,S/N=3)分别为0.15μg/kg、0.012μg/kg,定量限(LOQ,S/N=10)分别为0.5μg/kg、0.04μg/kg,回收率为82.6%~98.1%,相对标准偏差(RSD,n=6)为2.1%~8.1%。蔬菜、水果中BPA检出率分别为25%、18%,含量为0.172μg/kg~19.6μg/kg、0.164μg/kg~5.78μg/kg;BPS检出率分别为82%、76%,含量为0.012 6μg/kg~5.44μg/kg、0.012 8μg/kg~0.529μg/kg。结论该方法前处理简便、分析速度快、基质效应影响小、灵敏度高、准确性好,适用于蔬菜、水果中BPA、BPS同时测定。213份蔬菜、水果的测定结果表明,随着BPA的禁限用,BPS的应用日益广泛,相关部门有必要加大监管力度和执法范围,保障食品安全。

Objective A method for simultaneous determination of bisphenol A(BPA)and bisphenol S(BPS)in vegetables and fruits by isotope dilution-ultra performance liquid chromatography-triple quadrupole tandem mass spectrometry(UPLC-MS/MS)was established.Methods The samples were added with BPA and BPS isotope internal standard,acetonitrile ultrasonic extraction,GCB solid phase extraction column purification,methanol water gradient elution,ACQUITY UPLCTMBEH C18 column(100 mm×2.1 mm,1.7μm)separation,electrospray ionization source negative ion scanning(ESI-)multi reaction monitoring(MRM)mode determination,blank matrix matching standard curve,internal standard method quantitative.Results The linear ranges of BPA and BPS were within 0.5μg/L-20μg/L and 0.05μg/L-2.0μg/L,respectively.The correlation coefficients(r)were greater than 0.999.The detection limits(LOD,S/N=3)were 0.15μg/kg and 0.012μg/kg,respectively.The limits of quantification(LOQ,S/N=10)were 0.5μg/kg and 0.04μg/kg,respectively.The recoveries were within 82.6%-98.1%,and the relative standard deviations(RSD,n=6)were within 2.1%-8.1%.The detection rates of BPA in vegetables and fruits were 25%and 18%,with the content range of 0.172μg/kg-19.6μg/kg and 0.164μg/kg-5.78μg/kg;the detection rates of BPS were 82%and 76%,with the content range of 0.0126μg/kg-5.44μg/kg and0.0128μg/kg-0.529μg/kg,respectively.Conclusion The method is simple,rapid,sensitive and accurate.It is suitable for the simultaneous determination of BPA and BPS in vegetables and fruits.The results of 213 samples of vegetables and fruits showed that with the ban and restriction of BPA,the application of BPS was more and more extensive.It is necessary for relevant departments to strengthen supervision and law enforcement scope to ensure food safety.