离子色谱法测定白酒中10种阴离子

Determination of 10 anions in Baijiu by ion chromatography

采用离子色谱(IE)法测定白酒中10种阴离子(BrO_(3)^(-)、Cl^(-)、ClO_(3)^(-)、Br^(-)、NO_(3)^(-)、SO_(4)^(2-)、I^(-)、PO_(4)^(3-)、SCN^(-)、ClO_(4)^(-)),并进行方法学考察和23批白酒中10种阴离子的测定。结果表明,该检测方法分离度好(2.17~10.51),线性范围宽(I^(-)为0.5~10.0 mg/L、其他均为0.1~10.0 mg/L),线性相关性好(相关系数R>0.997)。重复性、精密度试验结果相对标准偏差(RSD)分别均<5%、<10%,除低加标量(2.5μg)条件下BrO_(3)^(-)和I^(-)加标回收率较差(分别36%和30%),其他8种阴离子(Cl^(-)、ClO_(3)^(-)、Br^(-)、NO_(3)^(-)、SO_(4)^(2-)、PO_(4)^(3-)、SCN^(-)、ClO_(4)^(-))的加标回收率为73%~128%,说明该方法的重复性、精密度、准确度较好。市售白酒中Cl^(-)、NO_(3)^(-)、SO_(4)^(2-)和PO_(4)^(3-)含量范围分别为0.5~15.0 mg/L、0.43~7.7 mg/L、0.3~33.0 mg/L、0.19~86.0 mg/L。BrO_(3)^(-)、ClO_(3)^(-)、SCN^(-)和ClO_(4)^(-)检出率分别为43%、56%、48%、9%,其中BrO_(3)^(-)和SCN^(-)最高检出分别为0.49 mg/L、1.20 mg/L,有潜在安全风险。综上,该方法能够应用于白酒中上述10种阴离子的测定。

The 10 anions(BrO_(3)^(-),Cl^(-),ClO_(3)^(-),Br^(-),NO_(3)^(-),SO_(4)^(2-),I^(-),PO_(4)^(3-),SCN^(-),ClO_(4)^(-))in Baijiu were determined by ion chromatography(IE),methodological investigation was carried out,and the content of 10 anions in 23 batches of Baijiu were determined.The results showed that the method had good resolution(2.17-10.51),wide linear range(I^(-)was 0.5-10.0 mg/L,other ions were 0.1-10.0 mg/L),and good linear correlation(correlation coefficient R>0.997).The relative standard deviation(RSD)of the repeatability and precision test results were less than 5%and less than 10%,respectively.Except for BrO_(3)^(-)and I^(-)with poor recovery rates(36%and 30%,respectively)under the low standard addition(2.5μg)conditions,the adding standard recovery of the other 8 anions(Cl^(-),ClO_(3)^(-),Br^(-),NO_(3)^(-),SO_(4)^(2-),PO_(4)^(3-),SCN^(-),ClO_(4)^(-))with standard addition was 73%-128%,indicating that the method had good repeatability,precision,and accuracy.The contents of Cl^(-),NO_(3)^(-),SO_(4)^(2-)and PO_(4)^(3-)in commercial Baijiu ranged from 0.5 to 15.0 mg/L,0.43 to 7.7 mg/L,0.3 to 33.0 mg/L,and 0.19 to 86.0 mg/L,respectively.The detection rates of BrO_(3)^(-),ClO_(3)^(-),SCN^(-)and ClO_(4)^(-)were 43%,56%,48%and 9%,respectively,and the highest detection content of BrO_(3)^(-)and SCN^(-)was 0.49 mg/L and 1.2 mg/L,respectively,indicating potential safety risks.In conclusion,the method could be applied to the determination of the above 10 anions in Baijiu.