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目的建立硫酸阿托品注射液有关物质新的测定方法,并研究有关物质和pH值之间的相关性。方法有关物质HPLC方法:Xbridge C_(18)柱(4.6 mm×250 mm,5μm);流动相A:庚烷磺酸钠磷酸盐溶液(含0.05 mol/L磷酸二氢钾溶液和0.002 5 mol/L庚烷磺酸钠溶液,用磷酸调节pH至3.9),流动相B:乙腈,梯度洗脱;流速:1 mL/min;检测波长210 nm,进样量为20μL。结果总杂质量与pH值大小成正相关。样品pH值在3.8~4.5间,总杂质量≥3.0%的占0.8%;在4.5~5.5间,总杂质量≥3.0%的有15.6%。结论杂质增大的主要原因为pH值的增大导致硫酸阿托品水解速度增加。pH值上限控制为4.5,可以提高合格率。
Objective To establish a new method for the determination of related substances of atropine sulfate injection and to study the correlation between related substances and pH value. Methods HPLC method: Xbridge C_ (18) column (4.6 mm × 250 mm, 5 μm); mobile phase A: sodium heptane sulfonate phosphate solution containing 0.05 mol / L potassium dihydrogen phosphate solution and 0.002 5 mol / L sodium heptanesulfonate solution, adjusted to pH 3.9 with phosphoric acid), mobile phase B: acetonitrile, gradient elution; flow rate: 1 mL / min; detection wavelength 210 nm, injection volume 20 μL. Results The total amount of impurities is positively correlated with the pH value. The sample pH was between 3.8 and 4.5, the total amount of impurities ≥ 3.0% accounted for 0.8%; 4.5 ~ 5.5, 15.6% of total impurities ≥ 3.0%. Conclusion The main reason for the increase of impurities is that the increase of pH value leads to the increase of hydrolysis rate of atropine sulfate. The upper limit of pH control is 4.5, which can improve the pass rate.