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目的建立二巯丁二酸中有关物质的HPLC测定方法。方法色谱柱为Ultimate XB-C18(4.6 mm×150 mm,5μm);流动相A:硫酸氢四丁基铵磷酸盐溶液(含硫酸氢四丁基铵3.2 g.L-1、磷酸二氢钠6.5 g.L-1和乙二胺四乙酸二钠0.09 g.L-1)-甲醇(85∶15),流动相B:甲醇;流速:1.0 mL.min-1;检测波长220 nm;线性梯度洗脱:0 min,100%A;10 min,100%A;20min,80%A;50 min,80%A。结果二巯丁二酸与丁炔二酸、各杂质峰之间分离良好。二巯丁二酸在14.0～112.0μg.mL-1内线性良好,r=0.999 3,检测限为1.8μg.mL-1;丁炔二酸在10.3～82.3μg.mL-1内线性良好,r=1.000 0,检测限为0.4μg.mL-1,丁炔二钠的平均加样回收率为98.3%。结论本方法专属性强、准确度高,适合测定二巯丁二酸的有关物质。
Objective To establish a HPLC method for the determination of related substances in thioglycerol. Methods The mobile phase A was tetrabutylammonium hydrogen sulfate solution (containing tetrabutylammonium hydrogen sulfate 3.2 gL-1, sodium dihydrogen phosphate 6.5 gL -1 and disodium ethylenediaminetetraacetate 0.09 gL-1) -methanol (85:15), mobile phase B: methanol, flow rate 1.0 mL.min-1, detection wavelength 220 nm, linear gradient elution 0 min , 100% A; 10 min, 100% A; 20 min, 80% A; 50 min, 80% A. Results 2-mercaptosuccinic acid and butylylenedioic acid, the impurity peaks separated well. The linear range of dithio-succinic acid was 14.0 ~ 112.0μg.mL-1, r = 0.999 3 and the limit of detection was 1.8μg.mL-1. Butynylacetic acid showed a good linearity in 10.3 ~ 82.3μg.mL-1, r = 1.000 0, the detection limit was 0.4μg.mL-1, and the average sample recovery of disodium butyne was 98.3%. Conclusion This method is highly specific and accurate and suitable for the determination of related substances of