使用一步水热合成法制备了二硫化钼-硫化镍（MoS₂-NiS）复合物，然后将此复合物滴涂在玻碳电极（GCE）上制备了MoS₂-NiS复合物修饰电极，记为MoS₂-NiS/GCE，用于饮用水和河水中亚硝酸盐含量的电化学测定。选择的电化学工作参数如下：①以MoS₂-NiS/GCE为工作电极，电解液为0.1 mol·L^-1磷酸盐缓冲溶液（pH 6）；②采用循环伏安法，扫描速率为50 mV·s^-1，电位范围为0.4~1.4 V。透射电子显微镜（TEM）和X射线衍射仪（XRD）表征结果表明：在复合材料中，棒状NiS附着在了片层状MoS₂表面，且复合物的XRD图谱中同时出现了NiS和MoS₂的衍射峰，说明已成功制备了MoS₂-NiS复合物。电化学试验结果表明：MoS₂-NiS/GCE的电催化性能明显优于单体制备的MoS₂/GCE和NiS/GCE的，且n_Mo/n_Ni=1：7的MoS₂-NiS/GCE的电催化效果较好；亚硝酸盐在MoS₂-NiS/GCE上的氧化受扩散过程控制。安培法检测结果表明，亚硝酸盐的浓度与其对应的氧化峰电流在0.9~1 210.0 μmol·L^-1内呈线性关系，检出限为0.25 μmol·L^-1。将该修饰电极在4℃下保存30 d后，氧化峰电流仅比初始值下降了7.4%。将该电极连续循环扫描20次，氧化峰电流的相对标准偏差为4.3%。用此修饰电极对饮用水和河水进行加标回收试验，所得回收率为97.4%~101%，测定值的相对标准偏差（n=5）为3.2%~4.5%，且所得测定值比国家标准GB/T 7493-1987的测定值更优异。

MoS₂-NiS composite was prepared by one-step hydrothermal synthesis method, and the modified glassy carbon electrode (labeled as MoS₂-NiS/GCE) was obtained by dropping the composite on GCE for electrochemical determination of nitrite content in drinking water and river water. The selected electrochemical working parameters were as follows: ① MoS₂-NiS/GCE was used as the working electrode, 0.1 mol·L^-1 phosphate buffer solution (pH 6) was used as the electrolyte; ② cyclic voltammetry was used as the analytical method under conditions of the scanning rate of 50 mV·s^-1 and the potential in the range of 0.4-1.4 V. The characterization results obtained by TEM and XRD showed that rod NiS adhered to the lamellar MoS₂ surface in the composite, and the diffraction peaks of NiS and MoS₂ appeared in the XRD pattern of the composite, indicating that the MoS₂-NiS composite had been successfully prepared. The results obtained by electrochemical test showed that the electrocatalytic performance of MoS₂-NiS/GCE was significantly superior to that of MoS₂/GCE and NiS/GCE prepared by monomer, and the electrocatalytic effect of MoS₂-NiS/GCE with n_Mo/n_Ni=1:7 was better. The oxidation of nitrite on MoS₂-NiS/GCE was controlled by diffusion process. Results of amperometric test showed that linearity relationship between concentration of nitrite and corresponding peak oxidation current was kept in the range of 0.9-1 210.0 μmol·L^-1, with detection limit of 0.25 μmol·L^-1. After placing the modified electrode at 4 ℃ for 30 d, the oxidation peak current decreased by 7.4% of the initial value. The modified electrode was scanned 20 times continuously, and RSD of oxidation peak currents was 4.3%. The modified electrode was used to analyze drinking water and river water in the spiked recovery test, giving recoveries in the range of 97.4%-101%, and RSDs (n=5) of determined values were ranged from 3.2% to 4.5%, with the determined values better than those of national standard GB/T 7493-1987.