RP-HPLC法定量测定呱西替柳中水杨酸愈创木酚酯和其有关物质HPLC-MS鉴别研究  被引量:4

Determination of Guaiacol salicylate in Guacetisal by HPLC method and qualitative identification of relevant substances by HPLC-MS

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作  者:孙国祥[1] 丁楠[1] 宋宇晴[1] 王真[1] 宋良伟 

机构地区:[1]沈阳药科大学药学院,沈阳110016 [2]山东罗欣药业股份有限公司,山东临沂276017

出  处:《中南药学》2010年第4期263-266,共4页Central South Pharmacy

摘  要:目的建立RP—HPLC法测定呱西替柳(GCTL)中水杨酸愈创木酚酯(GASAL)含量,用HPLGMS联用对GCTL中有关物质进行鉴别。方法用Agilent ZORBAX Eclipse XDB-C18柱(150mm×4.6mm,5μm);以甲醇-水(75:25)为流动相,流速1mL·min,柱温(30±0.15)℃,于检测波长为240nm定量测定CR2TL中GASAL含量,分别用超高效液相色谱质谱联用(UPLC-MS)和高效液相色谱飞行时间质谱联用(HPLGTOF-MS)鉴定有关物质。结果GASAL在3.0~100ng与峰面积呈良好线性关系,平均回收率为99.8%(RSD=1.53%)。在供试液中水杨酸愈创木酚酯随时间线性增加。HPLC-MS鉴别出6种有关物质分别可能是水杨酸、2-((2-甲氧基苯氧基)羰基)苯甲酚钠、2氧-2,3-苯并.2-氢呋喃7-羧酸-2-甲氧基苯酯、2-羟基苯甲酸-2-乙酰基苯酯、水杨酸愈创木酚酯、2-(2‘-乙酰氧基苯甲酰氧基)苯甲酸-2-甲氧基苯酯。结论测定GCTL中有关物质和GASAL含量应在制备样品溶液后20min内完成,GCTL中有关物质可能来自自身水解、酯化、内酯化及原料等。Objective To develop an RP HPLC method for the content determination of guaiacol salicylate (GASAL) in guacetisal (GCTL), and to identify relevant substances in GCTL by HPLC MS. Methods The operation was carried out on an Agilent ZORBAX Eclipse XDB-C18 column (150 mm×4.6 mm, 5 μm), with the mobile phase consisting of methanol-water (75 : 25). The flow rate was 1 mL · min ^-1 , the column temperature was (30±0. 15)℃ and the detection wavelength was 240 nm to quantitatively determine the content of GASAL in GCTL, and identify relevant substances by UPLC MS and HPLC-TOF-MS. Results The linear range for GASAL was 3.0- 100 ng and the mean recovery was 99.8% (RSD= 1.53%). The concentration of GASAL in solution increased linearly with time. The 6 relevant substances were 2 hydroxybenzoic acid; sodium 2 ((2-methoxyphenoxy) carbonyl) phenolate; 2-methoxyphenyl-2-oxo-2, 3-dihydrobenzofuran 7 carboxylate; and 2-acetylphenyl-2 hydroxybenzoate; 2-methoxyphenyl-2- hydroxybenzoate and 2- (2'-acetoxy-benzoyloxy) benzoic acid 2 methoxy-phenyl ester were identified by UPLC-MS and HPLC TOF MS. Conclusion Determination of relevant substances in GCTL and the content of GASAL should be completed within 20 min after the preparation of sample solution, and relevant substances in GCTL are mainly from hydrolysis, esterification, lactonization and guaicaol salicylate raw materials.

关 键 词:HPLC-MS HPLC-TOF-MS 呱西替柳 水杨酸愈创木酚酯 有关物质 

分 类 号:R927.2[医药卫生—药学]

 

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