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目的:建立同时测定果蔬中残留的噻苯咪唑(TBZ)、邻苯基苯酚(OPP)及联苯(DP)的 HPLC 法,并对乌鲁木齐地区部分高档水果中保鲜剂的残留状况进行初步评估。方法:在碱性条件下,用乙醚提取果蔬中 TBZ、OPP 及 DP 3种保鲜剂,以甲醇-乙腈-5 mmol·L~(-1)十二烷基磺酸钠溶液(磷酸调 pH:4.5)(55:10:35)为流动相,流速1.0 mL·min~(-1),荧光检测(λ_(ex)=285nm,λ_(em)=320 nm),进样量10μL。结果:TBZ、OPP 及 DP 的线性范围分别为0.01～8,0.007～10,0.01～20μg·mL~(-1);相关系数均大于0.999;最低检测限分别为0.01,0.007,0.01 μg·mL~(-1);平均回收率为71.4%～93.2%;RSD 为0.6%～6.5%。结论:本实验建立的 HPLC-荧光检测,方法准确可靠,适合于果蔬中噻苯咪唑、邻苯基苯酚及联苯残留的测定。
OBJECTIVE: To establish a HPLC method for the simultaneous determination of residual benzimidazole (TBZ), orthophenophenol (OPP) and biphenyl (DP) in fruits and vegetables, and to evaluate the residues of preservatives in some high-grade fruits in Urumqi. Methods: Three kinds of preservatives, TBZ, OPP and DP, were extracted from fruits and vegetables under alkaline conditions. The effects of methanol - acetonitrile - 5 mmol·L -1 sodium dodecyl sulfate on the pH, 4.5) (55:10:35) as the mobile phase at a flow rate of 1.0 mL · min ~ (-1), fluorescence detection (λ_ (ex) = 285 nm, λ_ (em) = 320 nm) Results: The linear range of TBZ, OPP and DP were 0.01 ~ 8,0.007 ~ 10,0.01 ~ 20μg · mL ~ (-1) respectively; the correlation coefficients were all greater than 0.999; the lowest detection limits were 0.01,0.007,0.01 μg · mL ~ (-1). The average recoveries ranged from 71.4% to 93.2%. The RSDs ranged from 0.6% to 6.5%. Conclusion: The HPLC-fluorescence detection method established in this experiment is accurate and reliable and suitable for the determination of thiophene imidazole, o-phenylphenol and biphenyl residues in fruits and vegetables.