摘要
目的建立高效液相色谱法同时测定盐酸羟甲唑啉鼻用制剂的有关物质和抑菌剂。方法 Agilent C_(18)(4.6 mm×250 mm,5 μm)色谱柱,磷酸缓冲液(pH=3)(A)-乙腈(B),梯度洗脱,流速1.0 mL·min^(-1),柱温30℃,检测波长214 nm,并以盐酸羟甲唑啉为参照物,采用斜率法初步计算杂质A的相对校正因子,并测定了17批市售制剂。结果杂质A的相对校正因子为1.43,校正因子法的计算值与外标法测定的结果一致。抑菌剂三氯叔丁醇和苯扎溴铵的检测质量浓度线性范围分别为1.511~5.756 mg·mL^(-1)和0.044~0.218 mg·mL^(-1),与峰面积线性关系良好(r^2>0.9999,n=6),定量限分别为89.95 ng和3.40 ng,检测限分别为35.98 ng和1.36 ng,加样回收率在95%~105%(RSD<2.0%,n=3),稳定性、重复性试验的RSD均<1.5%。结论本法灵敏度高,专属性好,可用于同时测定盐酸羟甲唑啉鼻用制剂的有关物质和抑菌剂。17批盐酸羟甲唑啉鼻用制剂的检测结果表明有必要增加有关物质和抑菌剂检测项。
Objective To simultaneously determine the related substances and bacteriostats in oxymetazoline hydrochloride nasal preparation by HPLC.Methods Agilent C18 column(4.6 mm×250 mm,5μm)was adopted.Potassium dihydrogen phosphate buffer(pH=3.0)and acetonitrile was used as the mobile phase with a gradient elution.The flow rate was 1.0 mL·min-1,the column temperature was maintained at 30℃,and the detection wavelength was 214 nm.The relative correction factor of impurity A was determined by HPLC with oxymetazoline hydrochloride as the internal standard.Totally 17 batches of commercial preparations were determined.Results The relative correction factor of impurity A was 1.43.The calculated value by the calibration factor method was consistent with the result determined by the external standard method.The linear ranges of chlorobutanol and benzalkonium bromide were 1.511~5.756 mg·mL-1,and 0.044~0.218 mg·mL-1;the limit of quantitation was 89.95 ng and 3.40 ng;and the limit of detection was 35.98 ng and 1.36 ng,respectively.Recovery was at 95%~105%(RSD<2.0%,n=3),RSDs of precision,stability and reproducibility were all lower than 1.5%.Conclusion The method has good sensitive and specificity,and suitable for the determination of related substances and bacteriostats in oxymetazoline hydrochloride nasal preparation simultaneously.It is necessary to add test items for related substances and bacteriostats.
作者
隋晓璠
刘慧颖
李尚颖
孙苓苓
SUI Xiao-fan;LIU Hui-ying;LI Shang-ying;SUN Ling-ling(Liaoning Province Inspection and Testing Certification Center,Liaoning Institute for Drug Control,Shenyang 110036)
出处
《中南药学》
CAS
2020年第7期1173-1178,共6页
Central South Pharmacy
基金
辽宁省自然基金资助计划(No.2020-MS-074)。
