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.
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.
Establishment of content determination of 5 saponins in Huoxue zhitong capsules/tablets and confirmation of illegal addition
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
>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.
关键词
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
Keywords
Huoxue zhitong tabletssaponinsPanax notoginsengPanax ginsengPanax quiquefoliumstems and leaves extract of Panax notoginsengillegal additionultra-high performance liquid chromatography tandem mass spectrometry