An HPLC and LC-MS Method for Analyzing 2,2′,4,4′,6,6′-Hexanitrostilbene

2,2′,4,4′,6,6′-hexanitrostilbene (HNS) is a heat-resistant, low-sensitivity energetic material with widespread applications in pliable linear-shaped charges, high-temperature-resistant oil well perforating charges, and rocket propellants. However, the presence of highly toxic and mutagenic nitroaromatic compounds in HNS wastewater necessitates efficient and accurate detection methods. Unfortunately, the existing analytical methods for HNS detection are outdated and incompatible with modern equipment. This limits their application due to issues with detection range, accuracy, and cost. To address this gap, an improved method was developed using an Ultimate 3000 UHPLC system with methanol and water as the mobile phase and UV-Vis detection at 271 and 226 nm wavelengths. The results indicate that the optimal detection conditions are achieved with a methanol-to-water ratio of 70:30 and a flow rate of 0.5 mL/min, providing high accuracy and efficiency. Compared to traditional methods, this approach reduced the detection time by nearly 70%, with the shortest analysis time ranging from 6 to 6.5 min, significantly lowering the cost of HNS detection. The method demonstrated excellent linearity (R2 > 0.9999) and high sensitivity within the concentration range of 0.50–150.00 mg/L, with precise and reliable results. This work provides both theoretical insights and experimental validation for the detection and analysis of HNS in wastewater.