高效液相色谱-内标法测定碘硝酚原料及其注射液中碘硝酚的含量  

Determination of Disophenol Content in Bulk Drug and Injection by High Performance Liquid Chromatography with Internal Standard Method

作　　者：孙婷婷[1] 田凯 王洪礼 杨杰[1] 田春莲[1] 刘明春[1] 牛生吏[1] SUN Ting-ting TIAN Kai WANG Hong-li YANG Jie TIAN Chun-lian LIU Ming-chun NIU Sheng-li(Institute of Animal Husbandry and Veterinary Medicine, Shenyang Agricultural University, Shenyang 110866, China Shenyang Viea Animal Husbandry Technology Limited Company, Shenyang 110027, China)

机构地区：[1]沈阳农业大学畜牧兽医学院,辽宁沈阳110866 [2]沈阳伟嘉牧业技术有限公司,辽宁沈阳110027

出　　处：《分析测试学报》2017年第8期1038-1042,共5页Journal of Instrumental Analysis

摘　　要：建立了碘硝酚的高效液相色谱(HPLC)-内标法检测方法。用甲醇将样品配制成测试浓度后过滤,经依利特Sino Chrom C_(18)(4.6 mm×200 mm,5μm)色谱分析柱进行色谱分离,流动相为0.02 mol/L磷酸二氢钾溶液(pH 2.6)-甲醇(30∶70),流速为1 mL/min,紫外检测波长为235 nm,柱温为30℃,内标物为硝氯酚,进样量为20μL。结果表明,碘硝酚的质量浓度在20~120 mg/L范围内呈线性关系,相关系数(r)为0.999 6;在3个不同浓度(64、80、96 mg/L)加标水平下,平均回收率为90.4%~98.2%,相对标准偏差(RSD)为0.18%~0.72%;检出限(LOD,S/N=3)为0.15 mg/L,定量下限(LOQ,S/N=10)为1.5 mg/L。该方法的精密度、稳定性以及重复性良好,且操作简便,结果准确,可用于碘硝酚原料药及注射液的含量测定。A simple and rapid method was developed for the determination of disophenol in bulk drug and injection via high performance liquid chromatography（HPLC） with the internal standard method. The sample was prepared with methanol to the test concentration, and filtrated with microfiltration membrane. Separation of analytes was achieved under isoeratic elution on a C18 column. The mobile phase consisted of a mixture of 0.02 moL/L potassium dihydrogen phosphate （pH 2.6） and methanol （30 ： 70） , and was delivered at a flow rate of 1 mL/min. The UV detection was set at 235 nm, and the column temperature was maintained at 30℃. The internal standard was nitroclofene and the injection volume was 20 μL. Under the optimum experimental conditions, the proposed HPLC - in- ternal standard method provided a good linearity in the range of 20 - 120 mg/L for disophenol with the correlation coefficients（r） of 0. 999 6. The average recoveries of disophenol at three spiked concen- tration levels of 64, 80 and 96 mg/L were in the range of 90. 4% - 98.2% , with relative standard deviations（RSDs） of 0. 18% -0.72%. The limits of quantitation（LOQs, S/N= 10） and limits of detection（LODs, S/N = 3） were 1.5 mg/L and 0. 15 rag/L, respectively. With good precision, stability and repeatability, the established method was simple, accurate, rapid and reliable for the determination of disophenol in bulk drug and injection.

关 键 词：碘硝酚 硝氯酚 含量测定 高效液相色谱法 内标法 

分 类 号：O657.72[理学—分析化学] O625.312[理学—化学]