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Determination of benzo(a)pyrene and aflatoxins (B1, B2, G1, G2) in vegetable oil by GPC-HPLC-FLD

机译:GPC-HPLC-FLD法测定植物油中的苯并(a)re和黄曲霉毒素(B1,B2,G1,G2)

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摘要

This study develops a gel permeation chromatography-high performance liquid chromatography-fluorescence detection (GPC-HPLC-FLD) method for determination of benzo(a)pyrene and aflatoxins (Bl, B2, Gl, G2) in vegetable oil. In the method, sample is extracted with ethyl acetate/cyclohexane (1:1, v/v), and cleaned up with the GPC. The separation of target compounds is performed on a Extend C_(18) column (4.6 × 250 mm, 5 μm) at 25 °C with methanol and 10 mmol L~(-1) ammonium acetate solution as mobile phase with gradient elution at a flow rate of 1.0 mL min~(-1). The injection volume was 10 μL, detection wavelengths were set at 360 nm (λ_(ex)) and 440 nm (λ_(em)) at 0-23 min, and 380 nm (λ_(ex)) and 408 nm (λ_(em)) at 23-35 min using FLD. The detection limits of benzo(a)pyrene and aflatoxins (B1, B2, G1, G2) were 0.5, 1.0, 1.0, 1.0 and 1.0 μg kg~(-1), respectively. The linear detection ranges of benzo(a)pyrene and aflatoxins (B1, B2, G1, G2) are 0.5-25.0 μg kg~(-1), 1.0-30.0 μg kg~(-1), 1.0-10.0 μg kg~(-1), 1.0-30.0 μg kg~(-1), 1.0-10.0 μg kg~(-1) with correlation coefficients (R~2) of 0.9998, 0.9999, 0.9997, 0.9998, 0.9996, respectively. Recovery rates in vegetable oil spiked with target compounds are in the range of 82.6-101.6%, with the relative standard deviation of 4.85-9.84%. The real sample tests show that this simple and accurate method can be used for determination of benzo(a)pyrene and aflatoxins (B1, B2, G1, G2) in vegetable oil.
机译:本研究开发了一种凝胶渗透色谱-高效液相色谱-荧光检测(GPC-HPLC-FLD)方法,用于测定植物油中的苯并(a)py和黄曲霉毒素(B1,B2,G1,G2)。在该方法中,样品用乙酸乙酯/环己烷(1:1,v / v)萃取,并用GPC净化。目标化合物的分离在25°C的Extend C_(18)色谱柱(4.6×250 mm,5μm)上以甲醇和10 mmol L〜(-1)乙酸铵溶液为流动相进行分离,并在流速为1.0 mL min〜(-1)。进样量为10μL,0-23分钟的检测波长分别设置为360 nm(λ_(ex))和440 nm(λ_(em)),以及380 nm(λ_(ex))和408 nm(λ_( em))在23-35分钟使用FLD。苯并(a)re和黄曲霉毒素(B1,B2,G1,G2)的检出限分别为0.5、1.0、1.0、1.0和1.0μgkg〜(-1)。苯并(a)re和黄曲霉毒素(B1,B2,G1,G2)的线性检测范围为0.5-25.0μgkg〜(-1),1.0-30.0μgkg〜(-1),1.0-10.0μgkg〜 (-1),1.0-30.0μgkg〜(-1),1.0-10.0μgkg〜(-1),相关系数(R〜2)分别为0.9998、0.9999、0.9997、0.9998和0.9996。加标有目标化合物的植物油中的回收率在82.6-101.6%的范围内,相对标准偏差为4.85-9.84%。实际样品测试表明,该简单而准确的方法可用于测定植物油中的苯并(a)re和黄曲霉毒素(B1,B2,G1,G2)。

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