浏览全部资源
扫码关注微信
1.南京医科大学药学院,南京 211112
2.南京市食品药品监督检验院,南京 211198
硕士研究生。研究方向:中药分析及质量评价。电话:025-89636150。E-mail:2322660686@qq.com
主任药师,硕士生导师,硕士。研究方向:中药分析及质量评价。电话:025-89636103。E-mail:2459437556@qq.com
纸质出版日期:2022-09-30,
收稿日期:2022-03-08,
修回日期:2022-07-06,
扫 描 看 全 文
陈洁,史达,曹玉等.活血止痛胶囊/片中5种皂苷类成分含量测定及确证非法添加方法的建立 Δ[J].中国药房,2022,33(18):2240-2244.
CHEN Jie,SHI Da,CAO Yu,et al.Establishment of content determination of 5 saponins in Huoxue zhitong capsules/tablets and confirmation of illegal addition[J].ZHONGGUO YAOFANG,2022,33(18):2240-2244.
陈洁,史达,曹玉等.活血止痛胶囊/片中5种皂苷类成分含量测定及确证非法添加方法的建立 Δ[J].中国药房,2022,33(18):2240-2244. DOI: 10.6039/j.issn.1001-0408.2022.18.13.
CHEN Jie,SHI Da,CAO Yu,et al.Establishment of content determination of 5 saponins in Huoxue zhitong capsules/tablets and confirmation of illegal addition[J].ZHONGGUO YAOFANG,2022,33(18):2240-2244. DOI: 10.6039/j.issn.1001-0408.2022.18.13.
目的
2
建立同时测定活血止痛胶囊/片中5种指标性皂苷类成分的含量和确证人参、西洋参、三七茎叶非法添加的方法。
方法
2
采用超高效液相色谱-串联质谱法。以Agilent RRHD Eclipse Plus C
18
为色谱柱,以水(含0.1%甲酸)-乙腈为流动相进行梯度洗脱,流速为0.35 mL/min,柱温为35 ℃,进样量为2 μL;采用电喷雾离子源,以多反应监测模式进行负离子扫描。
结果
2
三七皂苷R
1
、人参皂苷Rb
1
、人参皂苷Rg
1
、人参皂苷Rd、人参皂苷Re、人参皂苷Rf(人参特有成分)、人参皂苷Rb
3
(三七茎叶特有成分)、拟人参皂苷F
11
(西洋参特有成分)检测质量浓度的线性范围分别为9.99~1 499.50、9.99~1 499.50、10.01~1 500.80、9.99~1 499.10、10.00~1 500.20、9.99~1 499.50、10.01~1 500.80、9.99~1 499.00 ng/mL(
R
2
>0.997);检测限、定量限分别不高于2.64、8.06 ng/mL;精密度、重复性、稳定性(24 h)试验的RSD均小于6%;胶囊和片剂中各皂苷类成分的平均加样回收率分别为98.72%~102.40%、95.18%~106.47%(RSD均小于5%,
n
=6)。18批活血止痛胶囊中,三七指标性成分人参皂苷Re、人参皂苷Rd、人参皂苷Rg
1
、三七皂苷R
1
、人参皂苷Rb
1
的含量分别为291.79~426.89、427.71~677.49、2 294.28~3 371.43、571.22~848.19、1 841.33~2 959.12 μg/g,人参皂苷Rb
3
的含量均不高于45.02 μg/g;22批活血止痛片中,三七指标性成分的含量分别为44.11~393.83、80.48~549.55、393.36~3 548.57、79.83~872.60、288.64~2 912.66 μg/g,人参皂苷Rb
3
的含量不高于44.79 μg/g;2种制剂均未检出人参皂苷Rf、拟人参皂苷F
11
。
结论
2
该方法可用于测定活血止痛制剂中主要指标性皂苷类成分的含量。40批制剂均未见人参、西洋参非法添加现象,但部分批次片剂样品的三七药材投料量较少。
OBJECTIVE
2
To establish a method for simultaneous determination of 5 saponins in Huoxue zhitong capsules/tablets and to confirm the illegal addition of
Panax ginseng
,
Panax quiquefolium
and stems and leaves of
Panax notoginseng.
METHODS
2
Ultra-high performance liquid chromatography tandem mass spectrometry was used. The Agilent RRHD Eclipse Plus C
18
column was used with mobile phase of water (containing 0.1% formic acid)-acetonitrile for gradient elution at a flow rate of 0.35 mL/min. The column temperature was 35 ℃ and the sample size was 2 μL. Using electrospray ionization source, negative ion scanning was carried out in multi-reaction monitoring mode.
RESULTS
2
The linear ranges of notoginsenoside R
1
, ginsenoside Rb
1
, ginsenoside Rg
1
, ginsenoside Rd, ginsenoside Re, ginsenoside Rf(an unique ingredient of
P. ginseng
), ginsenoside Rb
3
(an unique ingredient of stems and leaves of
P. notoginseng
) and pseudo-ginsenoside F
11
(an unique ingredient of
P. quiquefolium
) were 9.99- 1 499.50, 9.99-1 499.50, 10.01-1 500.80, 9.99-1 499.10, 10.00-1 500.20, 9.99-1 499.50, 10.01-1 500.80, 9.99-1 499.00 ng/mL (
R
2
>0.997); the detection limits and the quantitative limits were not higher than 2.64 and 8.06 ng/mL, respectively. RSDs of precision, repeatability and stability (24 h) tests were all less than 6%. The average recoveries of saponins in capsules and tablets were 98.72%-102.40% and 95.18%-106.47%, respectively (all RSDs<5%,
n
=6). In 18 batches of Huoxue zhitong capsules, the contents of ginsenoside Re, ginsenoside Rd, ginsenoside Rg
1
, notoginsenoside R
1
and ginsenoside Rb
1
were 291.79-426.89, 427.71-677.49, 2 294.28-3 371.43, 571.22-848.19 and 1 841.33-2 959.12 μg/g, respectively; the contents of ginsenoside Rb
3
were no more than 45.02 μg/g. In 22 batches of Huoxue zhitong tablets, the contents of above indicators of
P. notoginseng
were 44.11-393.83, 80.48-549.55, 393.36-3 548.57, 79.83-872.60, and 288.64-2 912.66 μg/g, respectively; the contents of ginsenoside Rb
3
were no more than 44.79 μg/g. Ginsenoside Rf and pseudo-ginsenoside F
11
were not detected in the two preparations.
CONCLUSIONS
2
The method can be used to determine the contents of saponins in Huoxue zhitong preparations. No illegal addition of
P. ginseng
and
P. quiquefolium
are found in 40 batches of preparations, but the input of
P. notoginseng
in some batches of tablet samples is less.
活血止痛胶囊活血止痛片皂苷类成分三七人参西洋参三七茎叶提取物非法添加超高效液相色谱-串联质谱法
Huoxue zhitong tabletssaponinsPanax notoginsengPanax ginsengPanax quiquefoliumstems and leaves extract of Panax notoginsengillegal additionultra-high performance liquid chromatography tandem mass spectrometry
国家药典委员会.中华人民共和国药典:一部[S].2020年版.北京:中国医药科技出版社,2020:1392-1395.
国家药品监督管理局.国家药品标准:YBZ25062005-2010Z[S].2019版.北京:中国标准出版社,2019:1-2.
王晶,张勇,毕萌菲,等.RP-HPLC法分析测定人参、西洋参、三七中的皂苷类化合物[J].食品研究与开发,2020,41(7):172-176.
王峰,聂黎行,于健东,等.活血止痛制剂中三七的专属性鉴别方法研究[J].中国药事,2019,33(7):760-766.
赵振霞,王晓蕾,雷蓉,等.UPLC-MS/MS检测乌鸡白凤丸中非法添加西洋参[J].中国现代应用药学,2020,37(4):420-424.
赵振霞,王敏,王晓蕾,等.心可舒胶囊中非法添加三七茎叶的UPLC/MS/MS法检测[J].时珍国医国药,2019,30(3):619-622.
刘永利,赵振霞,苏建,等.三七粉质量评价研究[J].中国药事,2017,31(4):407-411.
刘永利,雷蓉,王晓蕾,等.基于中药质量标志物的人参、西洋参、三七及相关中成药质量控制方法研究[J].中国药学杂志,2019,54(17):1402-1410.
李丽,刘春明,吴巍,等.高效液相色谱-电喷雾质谱联用法测定人参和西洋参的皂苷类成分[J].分析化学,2005, 33(8):1087-1090.
刘鹏,王士伟,夏广萍.西洋参花蕾中人参皂苷Re、拟人参皂苷F11、人参皂苷Rb3、人参皂苷Rd的含量测定[J].中草药,2018,49(17):4144-4147.
刘翀,韩金玉,常贺英,等.三七茎叶提取物中人参皂苷Rb3的分离及指纹图谱[J].天津大学学报,2006, 39(10):1151-1156.
费毅琴,杨萍,肖凌,等.HPLC法快速筛查中成药中三七/人参茎叶代替根和根茎[J].中成药,2015,37(8):1730-1733.
袁铭铭,周国平,熊晓丽,等.高效液相色谱法测定虎力散片中三七皂苷R1、人参皂苷Rg1和Rb1的含量[J].药品评价,2021,18(21):1289-1292.
罗艳,杨柳,涂晓琴,等.高效液相色谱-蒸发光散射法同时测定山银花提取物中5种皂苷的含量[J].食品安全质量检测学报,2019,10(7):1914-1919.
洪艳,文晓霞,李莎,等. LC-MS/MS法同时测定复方丹参颗粒和复方丹参滴丸中6种成分[J].中成药,2019,41(2):270-274.
严华,张慧秀,白宗利,等.基于特征图谱的人参属药材西洋参、人参、三七的比较[J].世界中医药,2021,16(6):887-895.
0
浏览量
0
下载量
0
CSCD
关联资源
相关文章
相关作者
相关机构