CN104730193B - The detection method of volatile ingredient in a kind of WENXIN KELI - Google Patents

The detection method of volatile ingredient in a kind of WENXIN KELI Download PDF

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CN104730193B
CN104730193B CN201510145198.7A CN201510145198A CN104730193B CN 104730193 B CN104730193 B CN 104730193B CN 201510145198 A CN201510145198 A CN 201510145198A CN 104730193 B CN104730193 B CN 104730193B
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peaks
detection method
volatile ingredient
wenxin keli
wenxin
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CN104730193A (en
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吴红华
朱彦
赵步长
王忠平
赵涛
赵菁
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Shandong Buchang Pharmaceuticals Co Ltd
Tianjin University of Traditional Chinese Medicine
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Shandong Buchang Pharmaceuticals Co Ltd
Tianjin University of Traditional Chinese Medicine
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Abstract

The present invention provides the detection method of volatile ingredient in a kind of WENXIN KELI。The present invention adopts headspace solid-phase microextraction technology, extracts volatile ingredient in WENXIN KELI。And it is combined with gas chromatography-mass spectrometry technology, it is divided into from identifying volatile ingredient 74。10 batches of WENXIN KELI are analyzed, has drawn the relative amount scope of major volatile constituents。The present invention adopts headspace solid-phase microextraction in conjunction with GC-MS first; carry out extracting to volatile ingredient in WENXIN KELI and analyze; compensate for the deficiency in the past WENXIN KELI volatile material analyzed, the quality control for this medicine provides detection method more comprehensively。<!--2-->

Description

The detection method of volatile ingredient in a kind of WENXIN KELI
Technical field
The present invention relates to Chinese patent medicine detection method field, especially relate to the detection method of volatile ingredient in a kind of WENXIN KELI。
Background technology
WENXIN KELI, as conventional arrhythmia Chinese patent medicine, is mainly made up of medical materials such as Radix Codonopsis, Rhizoma Polygonati, Radix Notoginseng and Radix Et Rhizoma Nardostachyos, has supplementing QI and nourishing YIN, multiple arteries and veins of surely throbbing with fear, effect of blood circulation promoting and blood stasis dispelling。State approval code is: Z10950026。Cure mainly: deficiency of both QI and YIN is held concurrently the palpitation and uneasiness caused by heart arteries and veins stasis blocking, shortness of breath and fatigue, dizzy vexed, feeling of oppression and pain in the chest。The arrhythmia such as the premature beat that causes suitable in a variety of causes, atrial fibrillation, sinus tachycardia。Clinical practice is evident in efficacy。Except adjuvant, being mainly composed of polysaccharide, saponin and volatile ingredient (Radix et Rhizoma Nardostachyos volatile oil) in side, 2010 editions " Chinese Pharmacopoeia " records under WENXIN KELI item, it is stipulated that differentiate with Radix Codonopsis, Radix Notoginseng and Rhizoma Polygonati, with Panax Notoginseng saponin R1, ginsenoside Rg1And Rb1Total content carry out assay, the specification of the volatile ingredient being mainly derived from Radix Et Rhizoma Nardostachyos is not directed to。Radix Et Rhizoma Nardostachyos " makes medicine " at Fang Zhongwei, and clinical effect in arrhythmia and pharmacological mechanism report are more in recent years, increasingly receive publicity。The present invention at the clear and definite Radix Et Rhizoma Nardostachyos " status " in side, solve to have in the resource scarcity problem that faces and WENXIN KELI side is optimized is simplified etc. to be of great significance。
Headspace solid-phase microextraction (headspace-solidphasemicroextraction, HS-SPME) it is the novel sample pre-treatments risen the nineties in 20th century and beneficiation technologies, it it is a kind of extraction and separation technology with features such as rate of extraction are fast, simple to operate, bioaccumulation efficiency is high, required sample is few grown up on Solid-Phase Extraction (solidphaseextraction, SPE) basis。
Summary of the invention
The present invention provides the detection method of volatile ingredient in a kind of WENXIN KELI, it is therefore intended that, for the quality evaluation of WENXIN KELI, and it is the volatile ingredient quality control approach effectively in WENXIN KELI。
For solving above-mentioned technical problem, the detection method of volatile ingredient in a kind of WENXIN KELI provided by the invention, the present invention adopts headspace solid-phase microextraction technology to extract the volatile ingredient in WENXIN KELI, and utilizes gas chromatography-mass spectrography Analysis and Identification。
The detection method of the volatile ingredient in WENXIN KELI of the present invention, wherein said headspace solid-phase microextraction technical step is take WENXIN KELI, saturated sodium-chloride water solution, it is stirred, insert extracting head, extraction time 25~35min, take out, the volatile ingredient of gained will be extracted, injection gas chromatography instrument injection port, injector temperature 250 DEG C, desorption time 4~6min, sample introduction pattern is Splitless injecting samples, and utilizes gas chromatography-mass spectrography Analysis and Identification。
Preferably, the model of described extracting head is 100 μm of PDMS。
Preferably, described extraction time 30min。
Preferably, described desorption time 5min。
Preferably, described gas chromatography-mass spectrography Analysis and Identification condition is: chromatographic condition: HP-5MS, 60m × 320 μ m 0.25 μm;Carrier gas: He, flow 0.8mL/min;Vapourizing temperature: 250 DEG C;Interface temperature: 280 DEG C;Chromatographic column initial temperature 50 DEG C, keeps 1min, rises to 130 DEG C with 10 DEG C/min heating rate, keeps 6min, rise to 145 DEG C with 1 DEG C/min heating rate, keep 5min, rise to 160 DEG C with 1 DEG C/min heating rate, keep 3min, rise to 220 DEG C with 3 DEG C/min heating rate, keep 1min;
Mass Spectrometry Conditions: ionization mode: EI source, energy 70eV;Ion source temperature: 230 DEG C;Quadrupole rod temperature: 150 DEG C;Mass scan range: 35~800amu;Electron multiplier voltage: 1400V。
Further, according to above-mentioned set up assay method, measuring the finger printing that in WENXIN KELI, volatile ingredient obtains, have 19 common characteristic fingerprint peakses according in the finger printing that the method generates, the retention time obtained successively is: No. 1 peak is 10.78 ± 0.006min, No. 2 peaks are: 20.42 ± 0.007min, No. 3 peaks are: 21.03 ± 0.007min, No. 4 peaks are 21.39 ± 0.007min, No. 5 peaks are: 22.56 ± 0.008min, No. 6 peaks are 23.36 ± 0.009min, No. 7 peaks are: 24.71 ± 0.014min, No. 8 peaks are: 25.23 ± 0.012min, No. 9 peaks are: 26.11 ± 0.037min, No. 10 peaks are: 27.42 ± 0.022min, No. 11 peaks are: 34.80 ± 0.014min, No. 12 peaks are: 36.09 ± 0.018min, No. 13 peaks are: 37.25 ± 0.035min, No. 14 peaks are: 37.70 ± 0.048min, No. 15 peaks are: 40.85 ± 0.262min, No. 16 peaks are: 41.19 ± 0.053min, No. 17 peaks are: 44.29 ± 0.012min, No. 18 peaks are: 44.64 ± 0.014min, No. 19 peaks are: 60.81 ± 0.008min。
Further, according to above-mentioned set up assay method, measure the finger printing that in WENXIN KELI, volatile ingredient obtains, 19 common characteristic fingerprint peakses are had according in the finger printing that the method generates, wherein No. 1 peak is: Eucalyptol cineole, No. 2 peaks are: δ-EIemene δ-elemene, No. 3 peaks are: α-Cubebene α-cubebene, No. 4 peaks are: Tetracyclo [4.4.1.1 (7, 10) .0 (2, 5)] dodec-3-en-11-ol, No. 5 peaks are: α-Copaene α-capaene, No. 6 peaks are: β-Patchoulene β-patchoulene, No. 7 peaks are: Cadinene cadinene, No. 8 peaks are: (+)-Calarene Rhizoma Acori Calami alkene, No. 9 peaks are: (-)-Aristolene aristolene, No. 10 peaks are: Caryophyllene Flos Caryophylli alkene, No. 11 peaks are: Spathulenol spathulenol, No. 12 peaks are: Globulol globulol, No. 13 peaks are: (-)-Spathulenol (-)-spathulenol, No. 14 peaks are: the different aromadendrene epoxide of Isoaromadendreneepoxide, No. 15 peaks are: Humuleneepoxide2 oxalene epoxide 2, No. 16 peaks are: 1, 3a-Ethano (1H) inden-4-ol, octahydro-2, 2, 4, 7a-tetramethyl-, No. 17 peaks are: Widdrol widdrol, No. 18 peaks are: Patchoulialcohol patchouli alcohol, No. 19 peaks are: 4-(3, 3-Dimethyl-but-1-ynyl)-4-hydroxy-2, 6, 6-trimethylcyclohex-2-enone。
The present invention adopts the qualitative and quantitative analysis of volatile ingredient, process through chem workstation and from total ion current figure, calculate each component percentages by area normalization method, and chromatographic peak each in total ion current figure is calculated its KI value, utilize the mass spectrum that each chromatographic peak is corresponding to carry out the inspection of NIST08.L standard spectrum storehouse and determined each component。Measure through multiple batches of volatile component content, adopt preferred gas chromatography-mass spectrography analysis condition, the 10 batches of WENXIN KELI randomly drawed are analyzed, choose and represent peak and carry out statistical disposition。
Headspace solid-phase microextraction (headspace-solidphasemicroextraction, HS-SPME) has the advantages that rate of extraction is fast, simple to operate, bioaccumulation efficiency is high。
Technical solution of the present invention adopts headspace solid-phase microextraction and Gas chromatographyMass spectrometry (HS-SPME-GC-MS) WENXIN KELI to be extracted and has analyzed, and is divided into from determining 74 components, accounts for the 80.90% of total peak area。
The present invention adopts headspace solid-phase microextraction and Gas chromatographyMass spectrometry, and 10 batches of WENXIN KELI have been extracted and analyzed, and have chosen 19 and represents peak and carry out relative amount statistics, and 19 relative area sums representing peak are not less than the 40% of the gross area。
Beneficial effects of the present invention:
The present invention adopts headspace solid-phase microextraction carry out extracting to volatile ingredient in WENXIN KELI in conjunction with GC-MS and analyze first, by substantial amounts of experimentation, optimizes GC conditions-Mass Spectrometry Conditions。And the sample of 10 batches has been carried out content investigation, compensate for the deficiency in the past WENXIN KELI volatile material analyzed, also construct the GC/MS total ion current figure of WENXIN KELI volatile ingredient。The present invention adopts headspace solid-phase microextraction and Gas chromatographyMass spectrometry WENXIN KELI to be extracted and has analyzed, and is divided into from identifying volatile ingredient 74, accounts for the 80.90% of general volatile composition。The chemical composition and content thereof that objectively respond WENXIN KELI main volatile component can be compared, effectively characterize the quality of WENXIN KELI volatile ingredient。Further, the 10 batches of WENXIN KELI randomly drawed being analyzed, 19 that choose that separating degree is good, purity is high represent peak and carry out statistical disposition, it was found that the retention time at each peak and peak area are all more stable。This also illustrates the detection method that the present invention sets up, there is good repeatability and reliability, provide reliable approach for the quality control of volatile ingredient in WENXIN KELI。
Accompanying drawing explanation
Fig. 1 is the GC-MS total ion current figure of volatile ingredient in WENXIN KELI。
Fig. 2 is that in 10 batches of WENXIN KELI, the GC-MS total ion current of volatile ingredient stacks figure。
Fig. 3 is that 10 batches of WENXIN KELI represent chromatographic peak relative amount result。Wherein compound title respectively 1-Eucalyptol cineole representated by 19 chromatographic peaks in Fig. 3, 2-δ-EIemene δ-elemene, 3-α-Cubebene α-cubebene, 4-Tetracyclo [4.4.1.1 (7, 10) .0 (2, 5)] dodec-3-en-11-ol, 5-α-Copaene α-capaene, 6-β-Patchoulene β-patchoulene, 7-Cadinene cadinene, 8-(+)-Calarene Rhizoma Acori Calami alkene, 9-(-)-Aristolene aristolene, 10-Caryophyllene Flos Caryophylli alkene, 11-Spathulenol spathulenol, 12-Globulol globulol, 13-(-)-Spathulenol (-)-spathulenol, the different aromadendrene epoxide of 14-Isoaromadendreneepoxide, 15-Humuleneepoxide2 oxalene epoxide 2, 16-1, 3a-Ethano (1H) inden-4-ol, octahydro-2, 2, 4, 7a-tetramethyl-, 17-Widdrol widdrol, 18-Patchoulialcohol patchouli alcohol, 19-4-(3, 3-Dimethyl-but-1-ynyl)-4-hydroxy-2, 6, 6-trimethylcyclohex-2-enone。
Detailed description of the invention
In order to make those skilled in the art be better understood from technical scheme, below in conjunction with the drawings and the specific embodiments, technical scheme of the present invention is described in further detail。
1, the detection method of volatile ingredient in WENXIN KELI
A () headspace solid-phase microextraction extracts volatile ingredient:
By WENXIN KELI (Shandong Buchang Pharmaceutical Co., Ltd., 5g/ bag, product batch number: 1405023) 0.51g, analytical pure sodium chloride 3.6g and water 12mL put into 150ml ml headspace bottle, add stirrer, seal pad (containing transparent blue silica gel/PTFE pad) and aluminum cap, 70 DEG C of magnetic agitation, insert 100 μm of PDMS extracting head (Supelco, Bellefonte, Pa)。Making extracting head stretch out 1cm, extract 30min, take out, be immediately inserted into gas chromatograph injection port, injector temperature 250 DEG C, desorbing 5min, sample introduction pattern is Splitless injecting samples。
(b) gas chromatography-mass spectrography analysis condition:
Agilent7890A-5975CGC-MS gas chromatography mass spectrometry mass spectrograph (Agilent scientific & technical corporation of the U.S.), Chromatographic data system (MSDChemStationE.02.01, Agilent scientific & technical corporation of the U.S.);Chromatographic column: HP-5MS (60m × 320 μ m 0.25 μm);Carrier gas: He, flow 0.8mL/min;Vapourizing temperature: 250 DEG C;Interface temperature: 280 DEG C;Chromatographic column initial temperature 50 DEG C (keeps 1min), 130 DEG C (keeping 6min) are risen to 10 DEG C/min heating rate, 145 DEG C (keeping 5min) are risen to 1 DEG C/min heating rate, 160 DEG C (keeping 3min) are risen to 1 DEG C/min heating rate, rise to 220 DEG C with 3 DEG C/min heating rate, finally keep 1min。Ionization mode: EI source, energy 70eV;Ion source temperature: 230 DEG C;Quadrupole rod temperature: 150 DEG C;Mass range: (35~800) amu;Electron multiplier voltage: 1400V。
(c) KI pH-value determination pH:
Take n-alkane mixing reference substance (C8-C20, FLUKA company of the U.S., numbering: 04070,40mg/Linhexane) 0.8 μ L, by gas chromatography-mass spectrography analysis condition under above-mentioned steps (b) item, record each n-alkane retention time, adopt linear temperature increase formula to calculate the KI value of each component
KI = 100 n + 100 ( t x - t n ) t n + 1 - t n
In formula, tx, tn and tn+1 respectively analyzed component and carbon number are in n-alkane (tn < tx < tn+1) the eluting peak retention time (min) between n and n+1, and measurement result is in Table 1。
Table 1 n-alkane retention time
The qualitative and quantitative analysis of (d) volatile ingredient:
The GC-MS total ion current figure of WENXIN KELI volatile ingredient is shown in Fig. 1。
Process through chem workstation and from total ion current figure, calculate each component percentages by area normalization method, chromatographic peak each in total ion current figure is calculated its KI value, utilizing the mass spectrum that each chromatographic peak is corresponding to carry out the inspection of NIST08.L standard spectrum storehouse and determined each component, detailed results is in Table 2。
Volatile chemical component in table 2 WENXIN KELI
Note:: beyond n-alkane maximum retention time
The present invention adopts headspace solid-phase microextraction and Gas chromatographyMass spectrometry, and WENXIN KELI has been extracted and analyzed by (i.e. HS-SPME-GC-MS), is divided into from identifying volatile ingredient 74, accounts for the 80.90% of general volatile composition。
As seen from Table 2, in WENXIN KELI volatile ingredient be mainly different aromadendrene epoxide (11.71%), (-)-spathulenol (6.01%), 1,3a-Ethano (1H) inden-4-ol, octahydro-2,2,4,7a-tetramethyl-(5.08%), the sesquiterpenoids such as oxalene epoxide 2 (4.14%)。
E () multiple batches of volatile component content measures:
The present invention adopts headspace solid-phase microextraction and Gas chromatographyMass spectrometry, and the 10 batches of WENXIN KELI randomly drawed are analyzed, and 19 that choose that separating degree is good, purity is high represent peak and carry out statistical disposition, and the relative amount result of every batch is in Table 3。Test result indicate that: 19 peak areas of the volatile ingredient in 10 batches of WENXIN KELI and retention time are more stable。Carrying out statistical analysis after rejecting abnormalities value, show that WENXIN KELI represents retention time and the relative amount scope at peak, result is in Table 4。
GraphPadPrism5 software analysis WENXIN KELI represents peak relative amount result and sees Fig. 3。
Table 4 WENXIN KELI represents peak relative amount scope

Claims (7)

1. the detection method of volatile ingredient in a WENXIN KELI, it is characterized in that: described detection method adopts headspace solid-phase microextraction technology to extract the volatile ingredient in WENXIN KELI, and utilize gas chromatography-mass spectrography Analysis and Identification, wherein chromatographic condition: HP-5MS, 60m × 320 μ m 0.25 μm;Carrier gas: He, flow 0.8mL/min;Vapourizing temperature: 250 DEG C;Interface temperature: 280 DEG C;Chromatographic column initial temperature 50 DEG C, keeps 1min, rises to 130 DEG C with 10 DEG C/min heating rate, keeps 6min, rise to 145 DEG C with 1 DEG C/min heating rate, keep 5min, rise to 160 DEG C with 1 DEG C/min heating rate, keep 3min, rise to 220 DEG C with 3 DEG C/min heating rate, keep 1min;
Mass Spectrometry Conditions: ionization mode: EI source, energy 70eV;Ion source temperature: 230 DEG C;Quadrupole rod temperature: 150 DEG C;Mass scan range: 35~800amu;Electron multiplier voltage: 1400V。
2. detection method as claimed in claim 1, it is characterised in that: described headspace solid-phase microextraction technical step is take WENXIN KELI, saturated sodium-chloride water solution, it is stirred, insert extracting head, extraction time 25~35min, take out, the volatile ingredient of gained will be extracted, injection gas chromatography instrument injection port, injector temperature 250 DEG C, desorption time 4~6min, sample introduction pattern is Splitless injecting samples, and utilizes gas chromatography-mass spectrography Analysis and Identification。
3. detection method as claimed in claim 2, it is characterised in that: the model of described extracting head is 100 μm of PDMS。
4. detection method as claimed in claim 2, it is characterised in that: described extraction time 30min。
5. detection method as claimed in claim 2, it is characterised in that: described desorption time 5min。
6. the detection method as described in as arbitrary in claim 1-5, it is characterised in that having 19 common characteristic fingerprint peakses according in the finger printing that the method generates, the retention time obtained successively is: No. 1 peak is 10.78 ± 0.006min, No. 2 peaks are: 20.42 ± 0.007min, No. 3 peaks are: 21.03 ± 0.007min, No. 4 peaks are 21.39 ± 0.007min, No. 5 peaks are: 22.56 ± 0.008min, No. 6 peaks are 23.36 ± 0.009min, No. 7 peaks are: 24.71 ± 0.014min, No. 8 peaks are: 25.23 ± 0.012min, No. 9 peaks are: 26.11 ± 0.037min, No. 10 peaks are: 27.42 ± 0.022min, No. 11 peaks are: 34.80 ± 0.014min, No. 12 peaks are: 36.09 ± 0.018min, No. 13 peaks are: 37.25 ± 0.035min, No. 14 peaks are: 37.70 ± 0.048min, No. 15 peaks are: 40.85 ± 0.262min, No. 16 peaks are: 41.19 ± 0.053min, No. 17 peaks are: 44.29 ± 0.012min, No. 18 peaks are: 44.64 ± 0.014min, No. 19 peaks are: 60.81 ± 0.008min。
7. detection method as claimed in claim 6, it is characterized in that: have 19 common characteristic fingerprint peakses according in the finger printing that the method generates, wherein No. 1 peak is: Eucalyptol cineole, No. 2 peaks are: δ-EIemene δ-elemene, No. 3 peaks are: α-Cubebene α-cubebene, No. 4 peaks are: Tetracyclo [4.4.1.1 (7, 10) .0 (2, 5)] dodec-3-en-11-ol, No. 5 peaks are: α-Copaene α-capaene, No. 6 peaks are: β-Patchoulene β-patchoulene, No. 7 peaks are: Cadinene cadinene, No. 8 peaks are: (+)-Calarene Rhizoma Acori Calami alkene, No. 9 peaks are: (-)-Aristolene aristolene, No. 10 peaks are: Caryophyllene Flos Caryophylli alkene, No. 11 peaks are: Spathulenol spathulenol, No. 12 peaks are: Globulol globulol, No. 13 peaks are: (-)-Spathulenol (-)-spathulenol, No. 14 peaks are: the different aromadendrene epoxide of Isoaromadendreneepoxide, No. 15 peaks are: Humuleneepoxide2 oxalene epoxide 2, No. 16 peaks are: 1, 3a-Ethano (1H) inden-4-ol, octahydro-2, 2, 4, 7a-tetramethyl-, No. 17 peaks are: Widdrol widdrol, No. 18 peaks are: Patchoulialcohol patchouli alcohol, No. 19 peaks are: 4-(3, 3-Dimethyl-but-1-ynyl)-4-hydroxy-2, 6, 6-trimethylcyclohex-2-enone。
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