高效液相色谱法测定间硝基苯磺酸还原制备间氨基苯磺酸过程中的间氨基苯磺酸和间硝基苯磺酸
HPLC Determination of m-Aminobenzenesulfonic Acid and m-Nitrobenzenesulfonic Acid in the Preparation Process of m-Aminobenzenesulfonic Acid by Reduction of m-Nitrobenzenesulfonic Acid
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摘要: 提出了测定间硝基苯磺酸还原制备间氨基苯磺酸生产过程中间氨基苯磺酸和间硝基苯磺酸的高效液相色谱法。采用kromasil C18色谱柱(150 mm×4.6 mm,5 μm)分离,以0.10 mol·L-1的磷酸二氢铵溶液为流动相,紫外检测波长为236 nm。间氨基苯磺酸和间硝基苯磺酸的线性范围分别为4.0×10-5~2.4×10-4,8.0×10-5~4.0×10-4mol·L-1,检出限(3S/N)分别为1.5×10-6,3.5×10-6mol·L-1,测定下限(10S/N)分别为5.0×10-6,1.0×10-5mol·L-1。加标回收率在95.3%~102%之间,测定值的相对标准偏差(n=6)在0.86%~2.6%之间。Abstract: A HPLC method was proposed for determination of m-aminobenzenesulfonic acid and m-nitrobenzenesulfonic acid in the preparation process of m-aminobenzenesulfonic acid from reduction of m-nitrobenzenesulfonic acid. The analytes were separated on a kromasil C18 (150 mm×4.6 mm, 5 μm) chromatographic column, with ammonium dihydrogen phosphate solution (0.10 mol·L-1) as mobile phase, and detected at the UV wavelength of 236 nm. The linear ranges of m-aminobenzenesulfonic acid and m-nitrobenzenesulfonic acid were 4.0×10-5-2.4×10-4mol·L-1 and 8.0×10-5-4.0×10-4mol·L-1 respectively, with detection limits (3S/N) of 1.5×10-6mol·L-1 and 3.5×10-6mol·L-1, and the lower limits of determination (10S/N) of 5.0×10-6, 1.0×10-5mol·L-1, respectively. Recovery rates obtained by standard addition method were between 95.3% and 102% and RSDs (n=6) were in the range of 0.86%-2.6%.
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