目的 建立HPLC法測定氫氯噻嗪原料藥中有關物質。方法 采用Waters Symmetry C₁₈柱（250 mm×4.6 mm，5μm）；流動相A：0.02 mol/L磷酸二氫鉀溶液（用磷酸調pH值至3.2）–甲醇–四氫呋喃（94：6：1），流動相B：0.02 mol/L磷酸二氫鉀溶液（用磷酸調pH值至3.2）–甲醇–四氫呋喃（50：50：5）；梯度洗脫；檢測波長為224 nm；體積流量為1.0 mL/min；進樣量：20 μL；柱溫：35℃；樣品倉溫度：10℃。結果 氫氯噻嗪、4-氨基-6-氯-1，3-苯二磺酰胺、氯噻嗪線性范圍分別為0.030 06～6.011 00、0.030 01～6.002 00、0.030 08～6.015 00 μg/mL；4-氨基-6-氯-1，3-苯二磺酰胺、氯噻嗪的平均回收率分別為98.66%、99.17%，RSD值分別為1.53%、1.02%。結論 本法準確、可靠、專屬性強，可以控制氫氯噻嗪原料藥中有關物質，為質量標準提升提供參考。

Objective To develop a method for the determination of related substances in hydrochlorothiazide active pharmaceutical ingredients. Methods The analysis was performed on an Waters Symmetry C₁₈ column (250 mm×4.6 mm, 5 μm). The mobile phase A was 0.02 mol/L potassium phosphate monobasic buffer (pH 3.2)-methanol-tetrahydrofuran (94:6:1), and the mobile phase B was 0.02 mol/L potassium phosphate monobasic buffer (pH 3.2)-methanol-tetrahydrofuran (50:50:5) with gradient elution. The detection wavelength was 224 nm, the flow rate was 1.0 mL/min, injection volume was 20 μL, column temperature was 35℃, and sample temperature was set as 10℃. Results The calibration curve of hydrochlorothiazide, 4-amino-6-chlorobenzene-1,3-disulfonamide, and chlorothiazide were linear in the range of 0.030 06-6.011 00 μg/mL, 0.030 01-6.002 00 μg/mL, and 0.030 08-6.015 00 μg/mL. And the average recoveries were 98.66% and 99.17% and with RSD value of 1.53% and 1.02%, respectively. Conclusion The method is accurate, reliable, and specific for the determination of related substances in hydrochlorothiazide active pharmaceutical ingredients, which provides a reference for the improvement of quality standards.

R927.2