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1.辽宁中医药大学 药学院,辽宁 大连 116600
2.广西中医药大学 药学院,广西壮瑶药工程技术研究中心,南宁 530001
[第一作者] 张诗雯,在读硕士,从事中药炮制学研究,E-mail:13998300735@163.com
*高慧,博士,教授,从事中药炮制原理研究,Tel:0411-85890151,E-mail:gaohuitcm@163.com
收稿日期:2019-11-04,
网络出版日期:2020-01-14,
纸质出版日期:2020-04-20
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张诗雯, 张凡, 臧彬如, 等. UPLC-QqQ-MS/MS考察蒸制时长及压力对人参中皂苷类成分含量的影响[J]. 中国实验方剂学杂志, 2020,26(8):199-205.
Shi-wen ZHANG, Fan ZHANG, Bin-ru ZANG, et al. Effect of Steaming Time and Pressure on Contents of Six Ginsenosides in Ginseng Radix et Rhizoma by UPLC-QqQ-MS/MS[J]. Chinese journal of experimental traditional medical formulae, 2020, 26(8): 199-205.
张诗雯, 张凡, 臧彬如, 等. UPLC-QqQ-MS/MS考察蒸制时长及压力对人参中皂苷类成分含量的影响[J]. 中国实验方剂学杂志, 2020,26(8):199-205. DOI: 10.13422/j.cnki.syfjx.20200946.
Shi-wen ZHANG, Fan ZHANG, Bin-ru ZANG, et al. Effect of Steaming Time and Pressure on Contents of Six Ginsenosides in Ginseng Radix et Rhizoma by UPLC-QqQ-MS/MS[J]. Chinese journal of experimental traditional medical formulae, 2020, 26(8): 199-205. DOI: 10.13422/j.cnki.syfjx.20200946.
目的:
2
比较不同蒸制时长及压力对6种人参皂苷类成分总量的影响,确定红参的最佳炮制方法。
方法:
2
采用超高效液相色谱-三重四极杆串联质谱(UPLC-QqQ-MS/MS)对不同炮制工艺的红参中人参皂苷Rg
1
,Re,Rf,Rb
1
,Rc,Rb
2
进行含量测定,选择Waters ACQUITY UPLC BEH C
8
色谱柱(2.1 mm×100 mm,1.7 μm),流动相0.1%甲酸水溶液(A)-0.1%甲酸乙腈溶液(B)梯度洗脱(0~4 min,81%~79%A;4~6.3 min,79%~75%A;6.3~6.5 min,75%~71%A;6.5~9.5 min,71%A;9.5~16.5 min,71%~68.5%A;16.5~16.6 min,68.5%~60%A;16.6~19 min,60%~100%A),流速0.4 mL·min
-1
,柱温35 ℃;质谱分析采用电喷雾离子源(ESI),负离子采集模式,毛细管电离电压2.5 kV,脱溶剂气温度350 ℃,脱溶剂气流量700 L·h
-1
,锥孔气流量50 L·h
-1
,以多反应监测(MRM)模式采集,采集范围
m
/
z
100~1 500,其中人参皂苷Rg
1
,Re,Rf,Rb
1
,Rc,Rb
2
的定量离子对分别为
m
/
z
799.59~637.49,945.54~475.79,799.59~475.49,1 107.59~783.97,1 077.58~783.96,1 077.75~191.19。
结果:
2
蒸制时长为3 h时,各样品组6种人参皂苷类成分质量分数总和处于7.099 8~16.768 5 mg·g
-1
;常压蒸制时6种人参皂苷类成分总量为加压蒸制总和的2.5~12.6倍,明显优于加压蒸制。
结论:
2
在本实验条件下,红参的最佳炮制方式为鲜人参常压蒸制3 h。
Objective:
2
The processing method of red ginseng was determined by comparing the effects of different steaming time and pressure on the total content of six ginsenosides.
Method:
2
The contents of ginsenoside Rg
1
Re
Rf
Rb
1
Rc and Rb
2
were determined by ultra high performance liquid chromatography-triple quadrupole tandem mass spectrometry (UPLC-QqQ-MS/MS). The Waters ACQUITY UPLC BEH C
8
column (2.1 mm×100 mm
1.7 μm) was used. The mobile phase was 0.1% formic acid aqueous solution (A) and 0.1% formic acid acetonitrile solution (B) for gradient elution (0-4 min
81%-79%A; 4-6.3 min
79%-75%A; 6.3-6.5 min
75%-71%A; 6.5-9.5 min
71%A; 9.5-16.5 min
71%-68.5%A; 16.5-16.6 min
68.5%-60%A; 16.6-19 min
60%-100%A). The flow rate was set at 0.4 mL·min
-1
and the column temperature was set at 35 ℃. The mass spectrographic analysis employed electrospray ionization (ESI) and negative ion collection mode with capillary ionization voltage of 2.5 kV
desolvation temperature of 350 ℃
desolvation gas flow of 700 L·h
-1
and cone gas flow of 50 L·h
-1
. Multiple reaction monitoring (MRM) mode was used to collect information
the collection range was
m
/
z
100-1 500
detection was performed by MRM mode at
m
/
z
799.59-637.49 for ginsenoside Rg
1
m
/
z
945.54-475.79 for ginsenoside Re
m
/
z
799.59-475.49 for ginsenoside Rf
m
/
z
1 107.59-783.97 for ginsenoside Rb
1
m
/
z
1 077.58-783.96 for ginsenoside Rc
m
/
z
1 077.75-191.19 for ginsenoside Rb
2
.
Result:
2
When the steaming time was 3 hours
the total mass fraction of six ginsenosides in each sample group was 7.099 8-16.768 5 mg·g
-1
and the total amount of the six ginsenosides in atmospheric steaming was 2.5-12.6 times of that in pressurized steaming
which was obviously better than that in pressurized steaming.
Conclusion:
2
Under the conditions of this experiment
the best processing method of red ginseng is atmospheric steaming for 3 hours with fresh ginseng.
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