摘要
目的比较紫外-可见分光光度法和柱前衍生高效液相色谱法(HPLC)两种方法测定对乙酰氨基酚注射液中抗氧剂盐酸半胱氨酸的含量差异,研究盐酸半胱氨酸含量测定方法的可靠性。方法紫外-可见分光光度法:通过盐酸半胱氨酸与酸性茚三酮溶液反应生成红色产物,在559 nm波长处测定吸收度;柱前衍生HPLC:以2,4-二硝基氟苯为衍生化试剂,与对乙酰氨基酚注射液在60℃水浴暗处反应,HPLC测定。采用Agilent extend C_(18)(250 mm×4.6 mm,5μm)色谱柱,以乙腈-0.014 mol/L磷酸氢二钾溶液(用磷酸溶液调pH 8.2)(35:65)为流动相,流速1.0 mL/min,检测波长360 nm。结果使用紫外-可见分光光度法,测得3批样品的含量分别为0.24,0.24,0.23 mg/mL。使用柱前衍生HPLC,测得3批样品的含量分别为0.23,0.24,0.23 mg/mL。结论紫外-可见分光光度法和柱前衍生HPLC均可准确测定对乙酰氨基酚注射液中的抗氧剂盐酸半胱氨酸的含量。
Objective To investigate the diference between the contents of antioxidant cysteine hydrochloride in acetaminophen injection determined by UV-Vis spectrophotometry and HPLC with pre-column derivation. Methods A red colour product was produced by the reaction of cysteine hydrochloride and acidic-ninhydrin, and its absorbance at 559 nm was determined by UV-Vis spectrophotometry. Under the dark condition, 2, 4-dinitrofluorobenzene was used as derivatization reagent to react with acetaminophen injection at 60℃ in the water bath. Then HPLC was adopted to detect the content of cysteine hydrochloride. An Agilent extend C18 （250 mm× 4.6 mm, 5μm） column was used, with acetonitrile：0.014 mol/L dipotassium hydrogen phosphate solution （adjusted to pH 8.2 with phosphoric acid） （35：65） as mobile phase at a flow rate of 1.0 mL/min, and the detection wavelength was set at 360 nm. Results The contents of cysteine hydrochloride in three batches of acetaminophen injection tested by UV-Vis spectrophotometry and by HPLC with pre-column derivation were 0.24, 0.24, 0.23 mg/mL and 0.23, 0.24, 0.23 mg/mL, respectively. Conclusion The contents of cysteine hydrochloride in acetaminophen injection can be determined accurately by UV-Vis spectrophotometry and pre-column derivation HPLC.
作者
徐伟娜
刘林
李永贵
颜红
杨清华
XU Wei-na LIU Lin LI Yong-gui YAN Hong YANG Qing-hua(Shandong Provincial Key Laboratory of Biomedical Polymers, Shandong Academy of Pharmaceutical Sciences, Jinan 250101, China Shandong Provincial Key Laboratory of Mucosal and Transdermal Drug Delivery Technology, Shandong Freda Pharmaceutical Group Company, Jinan 250101, China)
出处
《食品与药品》
CAS
2017年第5期330-333,共4页
Food and Drug
