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1.江西中医药大学现代中药制剂教育部重点实验室,南昌 330004
2.萍乡市食品药品检验所,江西 萍乡 337000
3.西藏自治区食品药品检验研究院,拉萨 850000
主管中药师,硕士研究生。研究方向:中药学。E-mail:243348659@qq.com
教授,博士生导师,博士。研究方向:中药物质基础与质量评价。电话:0791-87118658。E-mail:kings2008@163.com
纸质出版日期:2023-04-15,
收稿日期:2022-10-31,
修回日期:2022-12-01,
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黄唤,易徐航,邱毅等.UPLC-MS/MS法同时测定不同基原藏黄堇中3种生物碱的含量 Δ[J].中国药房,2023,34(07):832-836.
HUANG Huan,YI Xuhang,QIU Yi,et al.Content determination of 3 alkaloids in different origins of Tibetan Corydalis pallida by UPLC-MS/MS[J].ZHONGGUO YAOFANG,2023,34(07):832-836.
黄唤,易徐航,邱毅等.UPLC-MS/MS法同时测定不同基原藏黄堇中3种生物碱的含量 Δ[J].中国药房,2023,34(07):832-836. DOI: 10.6039/j.issn.1001-0408.2023.07.12.
HUANG Huan,YI Xuhang,QIU Yi,et al.Content determination of 3 alkaloids in different origins of Tibetan Corydalis pallida by UPLC-MS/MS[J].ZHONGGUO YAOFANG,2023,34(07):832-836. DOI: 10.6039/j.issn.1001-0408.2023.07.12.
目的
2
建立并应用同时测定不同基原藏黄堇中荷包牡丹碱、原阿片碱、黄连碱含量的方法,为该类药材的基原确定和质量控制提供参考依据。
方法
2
采用超高效液相色谱-三重四极杆质谱联用(UPLC-MS/MS)法:色谱柱为Agilent EC-C
18
(100 mm×2.1 mm,2.7 μm),以乙腈-0.1%甲酸水溶液为流动相梯度洗脱,流速为0.2 mL/min,柱温为35 ℃。采用电喷雾离子源正离子模式检测,多反应监测扫描。
结果
2
荷包牡丹碱、原阿片碱、黄连碱的进样质量浓度分别在5.88~117.60、53.70~1 074.00、4.85~97.00 ng/mL之间与各自峰面积成良好的线性关系(
r
分别为0.998 2、0.991 9、0.999 6);定量限分别为2.35、1.07、1.46 ng/mL,检测限分别为1.17、0.54、0.49 ng/mL;精密度、稳定性(24 h)、重复性试验的RSD均未超过2.0%;平均加样回收率分别为97.41%、98.89%、105.44%(RSD均小于5.0%,
n
=6)。
结论
2
所建立的方法选择性好、准确度高,适用紫堇属植物中荷包牡丹碱、原阿片碱和黄连碱的快速分析。3种生物碱总量在不同基原药材中的含量从高到低依次为金球黄堇、尖突黄堇、矮黄堇、尼泊尔黄堇和斑花黄堇,其中金球黄堇和尖突黄堇中的生物碱含量比较接近,但斑花黄堇和尼泊尔黄堇中未检测到荷包牡丹碱。
OBJECTIVE
2
To establish and apply a method for simultaneous determination of the contents of dicentrine, protopine and coptisine in Tibetan
Corydalis pallida
of different origins, and to provide reference for origin determination and quality control of the kind of medicinal materials.
METHODS
2
Ultra performance liquid chromatography-tandem quadrupole mass spectrometry method was used. The determination was performed on Agilent EC-C
18
column (100 mm×2.1 mm, 2.7 μm) with mobile phase consisted of acetonitrile-0.1% formic acid by gradient elution. The flow rate was 0.2 mL/min, and the column temperature was set at 35 ℃. MS detection was carried out by electrospray ionization in positive modes, multiple reaction monitoring mode was used for quantitative analysis.
RESULTS
2
The injection mass concentrations of dicentrine, protopine, coptisine ranged from 5.88 to 117.60, 53.70 to 1 074.00, and 4.85 to 97.00 ng/mL, respectively, showing a good linear relationship with their respective peak areas (
r
=0.998 2, 0.991 9, and 0.999 6, respectively). The limits of quantitation were 2.35, 1.07 and 1.46 ng/mL; the limits of detection were 1.17, 0.54, 0.49 ng/mL, respectively. RSDs of precision, stability (24 h) and repeatability tests were all lower than 2.0%. The average recovery rates were 97.41%, 98.89% and 105.44% (all RSDs<5.0%,
n
=6).
CONCLUSIONS
2
The established method has good selectivity and high accuracy, and is suitable for the rapid analysis of dicentrine, protopine and coptisine in
Corydalis
. The total contents of three alkaloids in different original medicinal materials are from high to low in order of
C. chrysosphaera
,
C. mucronifera
,
C. pygmaea
,
C. hendersonii
and
C. conspersa
. The alkaloid contents in
C. chrysosphaera
and
C. mucronifera
are relatively similar, but no dicentrine has been detected in
C. conspersa
and
C. hendersonii
.
藏黄堇超高效液相色谱-三重四极杆质谱联用法荷包牡丹碱原阿片碱黄连碱含量测定
ultra performance liquid chromatography-tandem quadrupole mass spectrometry methoddicentrineprotopinecoptisinecontent determination
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易欢,彭芳,谢雨宸,等. HPLC-QqQ-MS法同时测定八味小檗皮胶囊中25种成分的含量[J]. 中国药房,2022,33(14):1682-1687.
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