摘要
目的采用超高效液相色谱-电喷雾三重四极杆质谱(UPLC-TQ-MS)技术建立了同时快速测定金红片(Jinhong Tablets)中12个成分(莽草酸、绿原酸、异绿原酸B、异绿原酸C、普洛托品、别隐品碱、延胡索乙素、紫堇碱、巴马汀、槲皮素、异川楝素、川楝素)的定量分析方法。方法采用Acquity UPLC BEH C18色谱柱(100 mm×2.1 mm,1.7μm),流动相为0.1%甲酸乙腈溶液-0.1%甲酸水溶液,梯度洗脱,体积流量为0.3mL/min;采用多反应监测模式同时对金红片中12个成分进行定量分析。结果在17 min内完成12个成分的准确定量;12个定量成分的线性范围分别为50.00~6 400.00μg/mL(r=0.999 1)、2.28~292.00μg/mL(r=0.999 9)、0.82~104.80μg/mL(r=0.999 8)、1.56~200.00μg/mL(r=0.999 7)、0.91~116.00μg/mL(r=0.999 0)、0.94~120.00μg/mL(r=0.999 0)、9.38~1 200.00μg/mL(r=0.997 4)、2.93~375.00μg/mL(r=0.999 0)、1.25~160.00μg/mL(r=0.999 9)、31.25~4 000.00μg/mL(r=0.999 7)、0.93~120.90μg/mL(r=0.999 8)、1.41~180.70μg/mL(r=0.999 7),平均加样回收率分别为101.9%、101.2%、97.9%、96.8%、100.8%、100.1%、108.7%、100.0%、99.2%、102.0%、99.0%、103.2%,15批金红片中12个成分的质量分数分别为10.11~22.72 mg/g、0.16~0.43 mg/g、0.06~0.23 mg/g、0.13~0.42 mg/g、0.08~0.26 mg/g、0.08~0.25 mg/g、1.94~2.59 mg/g、0.20~0.96 mg/g、0.07~0.30 mg/g、1.72~2.14mg/g、0.03~0.06mg/g、0.03~0.06mg/g。结论采用UPLC-TQ-MS所建立的多指标成分定量分析方法可适用于金红片中不同结构类型成分的同时检测,该方法简单、灵敏度高、专属性好,为金红片的整体质量控制研究提供参考和借鉴。
Objective To establish an effective UPLC-TQ-MS method for the simultaneous determination of 12 components(shikimic acid, chlorogenic acid, isochlorogenic acid B, isochlorogenic acid C, protopine, allocryptopine, tetrahydropalmatine, corydaline, palmatine, quercetin, isotoosendanin, and toosendanin) in Jinhong Tablets(金红片, JHT). Methods The chromatographic separation was performed on an Acquity UPLC BEH C18 column(100 mm × 2.1 mm, 1.7 μm) with a gradient elution of acetonitrile(0.1% formic acid) and water(0.1% formic acid), and the flow rate was set at 0.3 mL/min;Multiple reaction monitoring(MRM) mode was used for the quantification of 12 components. Results The 12 components were accurately quantified within 17 min, and the linear ranges of 12 quantitation components were 50.00—6 400.00 μg/mL(r = 0.999 1), 2.28—292.00 μg/mL(r = 0.999 9), 0.82—104.80 μg/mL(r = 0.999 8), 1.56—200.00 μg/mL(r = 0.999 7), 0.91—116.00 μg/mL(r = 0.999 0), 0.94—120.00 μg/mL(r = 0.999 0), 9.38—1 200.00 μg/mL(r = 0.997 4), 2.93—375.00 μg/mL(r = 0.999 0), 1.25—160.00 μg/mL(r = 0.999 9), 31.25—4 000.00 μg/mL(r = 0.999 7), 0.93—120.90 μg/mL(r = 0.999 8) and 1.41—180.70 μg/mL(r = 0.999 7). And the average recoveries were 101.9%, 101.2%, 97.9%, 96.8%, 100.8%, 100.1%, 108.7%, 100.0%, 99.2%, 102.0%, 99.0% and 103.2%, respectively. The contents of 15 batches of the 12 major components were in the ranges of 10.11—22.72 mg/g, 0.16—0.43 mg/g, 0.06—0.23 mg/g, 0.13—0.42 mg/g, 0.08—0.26 mg/g, 0.08—0.25 mg/g, 1.94—2.59 mg/g, 0.20—0.96 mg/g, 0.07—0.30 mg/g, 1.72—2.14 mg/g, 0.03—0.06 mg/g and 0.03—0.06 mg/g, respectively. Conclusion The multi-index components quantitative analysis method established by UPLC-TQ-MS is simple, sensitive and specific, it can be applied for the detection of ingredients with different structures, and provides a solid basis for overall quality control of JHT.
作者
刘苓娴
李海波
石丹枫
王振中
姚新生
肖伟
于洋
LIU Ling-xian;LI Hai-bo;SHI Dan-feng;WANG Zhen-zhong;YAO Xin-sheng;XIAO Wei;YU Yang(Institute of Traditional Chinese Medicine and Natural Products,Jinan University,Guangzhou 510632,China;State Key Laboratory of New-tech for Chinese Medicine Pharmaceutical Process,Kanion Pharmaceutical Co.,Ltd.,Lianyungang 222001,China)
出处
《中草药》
CAS
CSCD
北大核心
2021年第12期3552-3559,共8页
Chinese Traditional and Herbal Drugs
基金
国家自然科学基金重点项目(81630097)
热毒宁注射液标准化建设项目(ZYBZH-C-JS-31)。
关键词
UPLC-TQ-MS
金红片
质量控制
多反应监测
莽草酸
绿原酸
异绿原酸B
异绿原酸C
普洛托品
别隐品碱
延胡索乙素
紫堇碱
巴马汀
槲皮素
异川楝素
川楝素
UPLC-TQ-MS
Jinhong Tablets
quality control
multiple reaction monitoring
shikimic acid
chlorogenic acid
isochlorogenic acid B
isochlorogenic acid C
protopine
allocryptopine
tetrahydropalmatine
corydaline
palmatine
quercetin
isotoosendanin
toosendanin
