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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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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 (B1, B2, G1, 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 C18 column (4.6 ?— 250 mm, 5 ??m) at 25 ?°C with methanol and 10 mmol La?’1 ammonium acetate solution as mobile phase with gradient elution at a flow rate of 1.0 mL mina?’1. The injection volume was 10 ??L, detection wavelengths were set at 360 nm (??ex) and 440 nm (??em) at 0a€“23 min, and 380 nm (??ex) and 408 nm (??em) at 23a€“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 ??g kga?’1, respectively. The linear detection ranges of benzo(a)pyrene and aflatoxins (B1, B2, G1, G2) are 0.5a€“25.0 ??g kga?’1, 1.0a€“30.0 ??g kga?’1, 1.0a€“10.0 ??g kga?’1, 1.0a€“30.0 ??g kga?’1, 1.0a€“10.0 ??g kga?’1 with correlation coefficients (R2) 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 82.6a€“101.6%, with the relative standard deviation of 4.85a€“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。目标化合物的分离是在25℃下,在Extend C18色谱柱(4.6?-250 mm,5?m)上进行的,使用甲醇和10 mmol La?'1乙酸铵溶液作为流动相,并进行梯度洗脱。 1.0 mL最小值的速率1。进样量为10ΔL,检测波长设置为在0a-“ 23 min”处分别为360 nm(Δex)和440 nm(Δem),以及380 nm(Δex)和408 nm(Δex)。 em)在23a到35分钟之间使用FLD。苯并(a)py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1.0?g kga?-1。苯并(a)re和黄曲霉毒素(B1,B2,G1,G2)的线性检测范围为0.5a€“ 25.0?g kga?'1,1.0a?30.0 ?? g kga?'1,1.0a €“ 10.0 ?? g kga?'1,1.0a”“ 30.0 ?? g kga?'1,1.0a”“ 10.0 ?? g kga?'1”,相关系数(R2)为0.9998,0.9999,0.9997,0.9998 ,分别为0.9996。掺入目标化合物的植物油的回收率在82.6a±101.6%的范围内,相对标准偏差为4.85a±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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