超高效液相色谱法测定去痛片中4种成分的含量  

Determination of the four components contents in Qutong tablets by UPLC

作　　者：张媛媛 丁大中 李立 栾成章 

机构地区：[1]青岛市食品药品检验研究院,山东青岛266071

出　　处：《中国卫生检验杂志》2015年第19期3269-3271,共3页Chinese Journal of Health Laboratory Technology

摘　　要：目的建立去痛片中氨基比林、非那西丁、咖啡因和苯巴比妥的超高效液相色谱(UPLC)分析方法。方法将供试品用流动相超声提取,采用Waters ACQUITY UPLC BEH C18色谱柱(2.1 mm×100 mm,1.7μm),以0.05 mol/L磷酸二氢钾溶液-甲醇(55∶45,V/V)为流动相,检测波长为214 nm,流速为0.2 ml/min,柱温为30℃,进样体积为5μl。外标法峰面积定量。结果 4种成分在4 min内完成分离,线性范围为0.6μg/ml^210μg/ml,标准曲线的线性关系良好,相关系数(r)为0.999 2~0.999 5。检出限(S/N=3)为0.012 6 ng^0.035 7 ng,平均回收率为97.0%~100.3%,RSD为1.15%~1.55%。2批样品含量测定结果均符合国家标准规定。结论经验证,该方法简便、快速、分离效果好、灵敏度高,准确性和稳定性好,在日常检测中可大大降低检测成本,缩短检测周期,适用于去痛片中4种成分的含量测定。Objective To develop an ultra performance liquid chromatography（ UPLC） method for the determination of aminopyrine,phenacetin,caffeine and phenobarbital in Qutong tablets. Methods The samples were extracted with mobile phase-ultrasound,and then separated on Waters ACQUITY UPLC BEH C18column（ 2. 1 mm × 100 mm,1. 7 μm） with 0. 05 mol / L potassium dihydrogen phosphate solution- methanol（ 55∶45,V / V） as mobile phase at the flow rate of 0. 2 ml / min. The column temperature was set at 30 ℃,the detection wavelength was set at 214 nm and the injection volume was 5 μl. At last the samples were quantified by the peak area of external standard method. Results Four components were separated in 4 min and the UPLC method exhibited excellent linearity when it was among 0. 6 μg / ml- 210 μg / ml. The correlation coefficient was among 0. 999 2- 0. 999 5,the detection limits（ S / N = 3）,recovery rates and relative standard deviations（ RSD） of this method were 0. 012 6 ng- 0. 035 7 ng,97. 0%- 100. 3% and 1. 15%- 1. 55%,respectively. The results of the 2 batches of the samples were both complied with the national standards. Conclusion The analytical method is simple,rapid,accurate with high resolution and sensitivity and good stability,it can greatly reduce test cost,shorten the test cycle in the detection,and it is suitable for the determination of four components in Qutong tablets.

关 键 词：超高效液相色谱法 氨基比林 非那西丁 咖啡因 苯巴比妥 

分 类 号：R927.2[医药卫生—药学]