作　　者： ; ; ; ;

机构地区： 广东省药品检验所

出　　处： 《药学研究》 2019年第12期697-701,共5页

摘　　要： 目的建立感冒清片中南板蓝根的定性分析方法。方法采用高效液相色谱法,以2-苯并噁唑啉酮作为专属性指标成分对感冒清片中南板蓝根进行定性鉴别。色谱柱采用Agilent Ecilpse Plus C 18(4.6 mm×250 mm,5μm),以甲醇(A)-水(B)为流动相,梯度洗脱(0~40 min,20%A;40~60 min,20%A→70%A;60~80 min,70%A),流速为1.0 mL·min^-1,检测波长为271 nm,柱温为30℃,进样量为20μL。采用超高效液相色谱-四极杆串联飞行时间-质谱(UPLC-Q-TOF-MS)得到了2-苯并噁唑啉酮的分子离子峰,以此验证高效液相色谱法的鉴别结果。色谱柱采用Agilent Poroshell 120 EC-C 18(4.6 mm×50 mm,2.7μm),以乙腈(A)-0.1%甲酸溶液(B)为流动相,梯度洗脱(0~20 min,20%A→60%A;20~25 min,60%A),流速为0.2 mL·min^-1,检测波长为271 nm,柱温为30℃,进样量2μL;质谱采用电喷雾负离子模式采集数据,毛细管电压为3.5 kV,锥孔电压为65 V,离子源温度为150℃,扫描范围为m/z:50~300。结果通过对南板蓝根正品、伪品和混淆品共25批次样本进行比较,显示2-苯并噁唑啉酮为南板蓝根的专属性化学成分,以此作为指标成分建立的感冒清片中南板蓝根的定性分析方法具有专属性强、灵敏度高的特点。采用建立的方法对56批次感冒清片样品进行分析,仅有19批次检出2-苯并噁唑啉酮。结论该方法可用于感冒清片中南板蓝根的定性鉴别,同时为南板蓝根的质量控制奠定了研究基础。 Objective To establish a qualitative analysis method for Baphicacanthus cusiae in Ganmaoqing Tablets.Methods Qualitative identification of Baphicacanthus cusiae in Ganmaoqing Tablets was carried out by HPLC with 2-benzoxazolinone as specific index component.The separation was performed on Agilent Ecilpse Plus C 18(4.6 mm×250 mm,5μm)column,the mobile phase was composed of acetonitrile(A)and water(B)with gradient elution(0~40 min,20%A;40~60 min,20%A→70%A;60~80 min,70%A),the flow rate was 1.0 mL·min^-1,the detection wavelength was 271 nm,the column temperature was 30℃and the injection volume was 20μL.The molecular ion peaks of 2-benzoxazolinone were obtained in UPLC-Q-TOF-MS,thus to verify the identification results of HPLC.The separation was performed on a Agilent Poroshell 120 EC-C 18(4.6 mm×50 mm,2.7μm)column,the mobile phase was composed of acetonitrile(A)and 0.1%formic acid(B)with gradient elution(0~20 min,20%A→60%A;20~25 min,60%A),the flow rate was 0.2 mL·min^-1,the detection wavelength was 271 nm,the column temperature was 30℃and the injection volume was 2μL.The mass spectrometer was operated in the negative ion mode,the capillary voltage was 3.5 kV,the cone voltage was 65 kV,the ion source temperature was 150℃and the scanning range was m/z:50~300.Results By comparison of the test results of 25 genuine,counterfeit and adulterant samples of Baphicacanthus cusiae,2-benzoxazolinone was showed the specific chemical component of Baphicacanthus cusiae.The qualitative analysis method of Baphicacanthus cusiae in Ganmaoqing Tablets based on this index component had the characteristics of high specificity and sensitivity.The established method was used to analyze 56 batches of Ganmaoqing Tablets,and 2-benzoxazolinone was detected in 19 of them.Conclusion The method can be used for the qualitative identification of Baphicacanthus cusiae in Ganmaoqing Tablets,and simultaneusly provides research basis for the quality control of Baphicacanthus cusiae.

关 键 词： 感冒清片 南板蓝根 苯并噁唑啉酮 定性分析方法 高效液相色谱 超高效液相色谱 四级杆串联飞行时间 质谱

领　　域： []