CN105301158A - Fingerprint spectrum determination method for Simotang oral solution - Google Patents
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Abstract
The invention discloses a fingerprint spectrum determination method for a Simotang oral solution. The method comprises the steps that a solution to be tested is prepared; the chromatographic conditions are set in the mode that elastic quartz capillary columns are adopted as chromatographic columns, the program temperature is set in the mode that the initial temperature is set at 45 DEG C-60 DEG C (kept for 7 min), the temperature is increased to 65 DEG C-75 DEG C (kept for 10 min) at the speed of 2 DEG C-3 DEG C/min and then increased to 190 DEG C-210 DEG C at the speed of 2 DEG C-3 DEG C/min, the temperature of a vaporizing chamber is set at 245 DEG C-260 DEG C, an electrospray ion source (EI) is adopted as an ion source, and the mass range is set within 35-400 m/z; the structure of a component corresponding each peak is searched and identified according to a spectrum library, and calculation is performed on the chromatographic peaks through an area normalization method to get the percentages of all the components; determination is performed, wherein determination is performed by adopting a gas chromatography-mass spectrometry instrument, and a 70-min chromatogram map is recorded. The determination method has the advantages that qualitative and quantitative analysis is performed by combining a fingerprint spectrum technique with the gas chromatography-mass spectrometry instrument. The determination method is easy and convenient to operate, good in repeatability and stability and high in specificity. An obtained fingerprint spectrum is better in separation effect of all characteristic peaks and can serve as a standard fingerprint spectrum for determining the ingredients of the Simotang oral solution to identify the effective ingredients of the Simotang oral solution.
Description
Technical field
The invention belongs to technical field of medicine quality control, particularly a kind of fingerprint atlas detection method of oral mushroom liquor, and obtain its standard finger-print thus.
Background technology
Decoction of Four-Drug Juice is made up of the banksia rose, betel nut, Fructus Aurantii, the root of three-nerved spicebush 4 taste medicinal material.The party mainly have pleasant fall inverse, disappear effect of long-pending pain relieving, be usually used in stagnant card in infant's breast food, that disease is seen abdominal distension, suffered from abdominal pain, uneasiness of crying, apocleisis are received is poor, diarrhoea or constipation, person in middle and old age's stagnation of the circulation of vital energy, dyspepsia are demonstrate,proved, disease sees abdominal fullness and distention, stomachache, constipation, and abdominal postoperative promotes the recovery of functions of intestines and stomach.Apply comparatively extensive clinically.
Monarch drug in a prescription in the banksia rose side of being in decoction of Four-Drug Juice, main containing volatile oil composition, this constituents is the principal ingredient that the banksia rose plays promoting qi circulation and relieving pain, reinforcing spleen to promote digestion effect, also has the effect of relaxing smooth muscle and spasmolysis simultaneously.
Oral mushroom liquor is as Chinese patent drug, and its drug effect is the coefficient result of various active composition.The existing quality standard of current oral mushroom liquor is WS-10040-(ZD-0040)-2002, only measure the content of single index components aurantiin, other effective constituents are not monitored, there is certain limitation, the quality level of oral mushroom liquor can not be reflected comprehensively.Publication for the quality determining method of oral mushroom liquor only has two, Chinese patent 201110074548.7(publication number CN102221590A) adopt HPLC method to control the content of its synephrine, norisoboldine and arecaline, Chinese patent 201110125049.6(publication number CN102346177A) adopt HPLC method structure finger-print to control its quality.As follows for the quality determining method of oral mushroom liquor through report, have recorded in " Chinese Pharmaceutical Affairs " the 28th volume the 3rd phase in 2014 " oral mushroom liquor quality standard Supplementary Study " and measure synephrine in oral mushroom liquor by HPLC method, norisoboldine, arecaline, aurantiin, new city skin glycosides content, " medical Leader " volume supplementary issue June the 28th in 2009 " content of high effective liquid chromatography for measuring naringin in Simotang oral solution ", a kind of HPLC method measuring naringin in Simotang oral solution content is described in the articles such as volume the 4th phase in " Bethune medical academy journal " August the 8th in 2010 " improvement of high effective liquid chromatography for measuring naringin in Simotang oral solution content method ", volume the 4th phase in " Hunan University of Traditional Chinese Medicine's journal " August the 29th in 2009 content of arecaline " in the high effective liquid chromatography for measuring oral mushroom liquor " describes a kind of HPLC method measuring arecaline content in oral mushroom liquor, " Chinese Medicine guide " the 11st volume the 1st phase in 2009 " HPLC method measures the content of synephrine in oral mushroom liquor " describes a kind of HPLC method measuring synephrine content in oral mushroom liquor.In prior art, although control the many index composition of oral mushroom liquor, but there is no the method control effectively to its volatile ingredient, the fingerprint atlas detection method therefore set up for volatile ingredient has very important significance to the quality controlling oral mushroom liquor.
Summary of the invention
The object of this invention is to provide a kind of fingerprint atlas detection method of oral mushroom liquor, the volatile ingredient in oral mushroom liquor can be controlled by this assay method thus control its quality, to ensure its clinical efficacy.
The present invention is a kind of fingerprint atlas detection method of oral mushroom liquor, it is characterized in that the method adopting gas chromatography mass spectrometry detects, comprises the following steps:
(1) preparation of need testing solution: get oral mushroom liquor, extracts with volatile oil extractor, obtains need testing solution;
(2) GC conditions: chromatographic column is fused-silica capillary column; Chromatographic column temperature programme condition: initial temperature 45-60 DEG C (keeping 7min), is warming up to 65-75 DEG C (keeping 10min) with 2-3 DEG C/min, then is warming up to 190-210 DEG C with 2-3 DEG C/min; Vaporizer temperature 245-260 DEG C; Carrier gas is high-purity helium; Carrier gas flux is 1.53mL/min; Sample size is 0.1 μ L; Split ratio is 1:50;
(3) Mass Spectrometry Conditions: ion gun is electric spray ion source (EI), and ion source temperature is 220 ~ 240 DEG C; Electron energy is 70ev; Mass range is 35-400m/z;
(4) measure: adopt gas chromatography mass spectrometry to measure; Draw need testing solution, injection gas chromatography-GC-MS, measure, record 70min chromatogram, obtains finger-print.
In the present invention, the preparation method of described need testing solution adopts volatile oil extractor to extract 2 ~ 4h, and preferred extraction time is 3h.
In the present invention, described chromatographic column is fused-silica capillary column, and preferred chromatographic column is to be cross-linked 5% methyl-polysiloxane for Stationary liquid.
In the present invention, described preferred chromatographic column temperature programme condition is: initial temperature 50 DEG C (keeping 7min), is warming up to 70 DEG C (keeping 10min), then is warming up to 200 DEG C with 2.5 DEG C/min with 2.5 DEG C/min.
In the present invention, described vaporizer temperature 250 DEG C; Carrier gas is high-purity helium; Carrier gas flux 1.53mL/min; Split ratio 1:50.
In the present invention, the accurate sample size drawing the need testing solution of inject gas chromatograph is 0.1 μ l.
In the present invention, gas chromatograph-mass spectrometer is adopted to measure; Draw need testing solution, injection gas chromatography-GC-MS, measure, record 70min chromatogram, identify the structure of the corresponding component in each peak according to library searching, and chromatographic peak area normalization method is calculated, ask for the percentage composition of each component, with No. 5 peak alpha-terpineols for reference peak, calculate relative retention time.
In the present invention, in the finger-print of described oral mushroom liquor, single peak area all exceedes total peak area 1% and determines that the total peak of composition has 8, the composition determined is as follows: No. 1 peak is cis-α, α-5-trimethyl-5-vinyl tetrahydrofuran-2-methyl alcohol, No. 2 peaks are trans linalool oxide, No. 3 peaks are linalool, No. 4 peaks are (R)-(-)-4-terpilenol, No. 5 peaks are alpha-terpineol, No. 6 peaks are geraniol, No. 7 peaks are inner mold-1,3,3-trimethyl two ring [2.2.1] heptane-2-alcohol acetic ester, No. 8 peaks are leukotrienes.
In the present invention, the total peak that in the finger-print of described oral mushroom liquor, single peak area all exceedes total peak area 1% has 8, with No. 5 peak alpha-terpineols for reference peak, calculate relative retention time, the relative retention time at each peak is respectively: (1) 0.523 ~ 0.641, (2) 0.564 ~ 0.689, (3) 0.610 ~ 0.789, (4) 0.825 ~ 0.970, (5) 1.000, (6) 1.266 ~ 1.548, (7) 1.313 ~ 1.618, (8) 2.665 ~ 3.035; Preferred each peak relative retention time is respectively: (1) 0.567 ~ 0.601, (2) 0.594 ~ 0.641, (3) 0.621 ~ 0.761, (4) 0.865 ~ 0.930, (5) 1.000, (6) 1.342 ~ 1.494, (7) 1.353 ~ 1.548, (8) 2.765 ~ 2.914.
Advantage of the present invention is as follows:
(1) banksia rose in oral mushroom liquor, Fructus Aurantii contain more volatile ingredient, but do not control it in existing quality standard, the gas chromatography mass spectrometry finger-print being Index Establishment with the volatile ingredient in oral mushroom liquor effectively can characterize the quality of oral mushroom liquor;
(2) the present invention has good stability, favorable reproducibility, feature that precision is high.
Below in conjunction with preferred forms and accompanying drawing, the present invention is further explained, the present invention is not construed as limiting.
Accompanying drawing explanation
Fig. 1 is 10 batch sample trace analysis, and spectrogram is basically identical shows that active constituent content is basically identical.
Fig. 2 reference fingerprint.
the structure of embodiment-oral mushroom liquor finger-print
Below by specific embodiment, the invention will be further described, and this embodiment, only for illustration of the present invention, does not limit the scope of the invention.
(1) instrument and reagent
Shimadzu QP2010UItra type GC/MS gas chromatograph-mass spectrometer and GCMSsolutions workstation;
HP-5MS quartz capillary column (30m × 0.25mm × 0.25 μm), Anjelen Sci. & Tech. Inc;
MEGA-5MS quartz capillary column (30m × 0.25mm × 0.25 μm), Italian Mai Ge chromatogram company;
Oral mushroom liquor (producer: HuNan HanSen Pharmacy Co., Ltd, lot number: 1408210,1408211,1408212,1408310,1408309,1407205,1404306,1404302,1404309,1404318).
(2) selection of chromatographic condition.
The selection of heating schedule
Due to complicated component in sample, need grope heating schedule, when heating up by following program, in sample, each component all has good separation, and baseline is steady, therefore selects this heating schedule as optimum temperature rise program.Heating schedule is as follows: initial temperature 50 DEG C (keeping 7min), is warming up to 70 DEG C (keeping 10min), then is warming up to 200 DEG C with 2.5 DEG C/min with 2.5 DEG C/min.
The selection of chromatographic column
By comparing HP-5MS quartz capillary column (30m × 0.25mm × 0.25 μm), MEGA-5MS quartz capillary column (30m × 0.25mm × 0.25 μm), the chromatographic column of 2 kinds of different brands, result shows, it is moderate that the chromatographic column of above 2 kinds of brands all can reach retention time, peak number order is more, the comparatively ideal chromatogram effect that degree of separation is good.
The selection of different carrier gas flux
When other chromatographic conditions are identical, investigating carrier gas flux is respectively the impact that 1.33ml/min, 1.53ml/min, 1.73ml/min are separated same sample chromatographic peak.Result shows, when carrier gas flux is 1.53ml/min, chromatographic peak retention time is moderate, and degree of separation is best, and repeatability is best.
(3) preparation of need testing solution.
Get oral mushroom liquor 2L, extract 3h with volatile oil extractor, obtain need testing solution.
(4) methodological study.
Stability test
Get same need testing solution, under these conditions, detect respectively at 0,2,4,6,12,24 hour, each sample introduction 0.1 μ l, investigates the relative retention time of main chromatographic peak and the consistance of relative peak area.The relative retention time of the main chromatographic peak of result and the RSD < 3% of relative peak area, show in need testing solution 24 hours more stable.
Precision test
Get with a need testing solution, under these conditions, repeat sample introduction 6 times, each sample introduction 0.1 μ l, investigates the relative retention time of main chromatographic peak and the consistance of relative peak area.The relative retention time of the main chromatographic peak of result and the RSD < 3% of relative peak area, show that instrument precision is good.
Replica test
Get with a collection of decoction of Four-Drug Juice sample, prepare 6 parts of need testing solutions by test sample preparation method, under these conditions, sample introduction analysis, investigates the relative retention time of main chromatographic peak and the consistance of relative peak area.The relative retention time of the main chromatographic peak of result and the RSD < 3% of relative peak area, show that the method is reproducible.
(5) formulation of oral mushroom liquor standard finger-print.
The above-mentioned need testing solution 0.1 μ l of accurate absorption, sample introduction analysis, record spectrogram; According to the finger-print of 10 batches of oral mushroom liquors of gained, formulate standard finger-print.See Fig. 1,2.
Relatively oral mushroom liquor chromatogram, the total peak that single peak area all exceedes total peak area 1% has 8, and wherein No. 5 peaks are alpha-terpineol, according to " technical requirement of traditional Chinese medicine finger-print research ", formulates the standard finger-print of Shensu Oral Liquid".With alpha-terpineol peak for reference peak, calculate the relative retention time at each peak.
The relative retention time at each peak is respectively: (1) 0.567 ~ 0.601, (2) 0.594 ~ 0.641, (3) 0.621 ~ 0.761, (4) 0.865 ~ 0.930, (5) 1.000, (6) 1.342 ~ 1.494, (7) 1.353 ~ 1.548, (8) 2.765 ~ 2.914.
(6) similarity evaluation.
Table 110 batch oral mushroom liquor fingerprint similarity evaluation result table
| S1 | S2 | S3 | S4 | S5 | S6 | S7 | S8 | S9 | S10 | Contrast collection of illustrative plates | |
| S1 | 1.000 | 0.945 | 0.988 | 0.967 | 0.984 | 0.812 | 0.803 | 0.901 | 0.941 | 0.947 | 0.976 |
| S2 | 0.945 | 1.000 | 0.944 | 0.925 | 0.916 | 0.914 | 0.877 | 0.861 | 0.946 | 0.952 | 0.970 |
| S3 | 0.988 | 0.944 | 1.000 | 0.943 | 0.904 | 0.952 | 0.845 | 0.831 | 0.936 | 0.899 | 0.957 |
| S4 | 0.967 | 0.925 | 0.943 | 1.000 | 0.969 | 0.917 | 0.974 | 0.962 | 0.911 | 0.907 | 0.974 |
| S5 | 0.984 | 0.916 | 0.904 | 0.969 | 1.000 | 0.978 | 0.964 | 0.926 | 0.924 | 0.914 | 0.947 |
| S6 | 0.812 | 0.914 | 0.952 | 0.917 | 0.978 | 1.000 | 0.966 | 0.914 | 0.971 | 0.917 | 0.988 |
| S7 | 0.803 | 0.877 | 0.845 | 0.974 | 0.964 | 0.966 | 1.000 | 0.978 | 0.874 | 0.948 | 0.951 |
| S8 | 0.901 | 0.861 | 0.831 | 0.962 | 0.926 | 0.914 | 0.978 | 1.000 | 0.858 | 0.984 | 0.952 |
| S9 | 0.941 | 0.946 | 0.936 | 0.911 | 0.924 | 0.971 | 0.874 | 0.858 | 1.000 | 0.920 | 0.965 |
| S10 | 0.947 | 0.952 | 0.899 | 0.907 | 0.914 | 0.917 | 0.948 | 0.984 | 0.920 | 1.000 | 0.986 |
| Contrast collection of illustrative plates | 0.976 | 0.970 | 0.957 | 0.974 | 0.947 | 0.988 | 0.951 | 0.952 | 0.965 | 0.986 | 1.000 |
Claims (9)
1. the present invention is a kind of fingerprint atlas detection method of oral mushroom liquor, it is characterized in that the method adopting gas chromatography mass spectrometry detects, comprises the following steps:
A the preparation of () need testing solution: get oral mushroom liquor, extracts with volatile oil extractor, obtains need testing solution;
(b) GC conditions: chromatographic column is fused-silica capillary column; Chromatographic column temperature programme condition: initial temperature 45-60 DEG C (keeping 7min), is warming up to 65-75 DEG C (keeping 10min) with 2-3 DEG C/min, then is warming up to 190-210 DEG C with 2-3 DEG C/min; Vaporizer temperature 245-260 DEG C; Carrier gas is high-purity helium; Carrier gas flux is 1.53mL/min; Sample size is 0.1 μ L; Split ratio is 1:50;
(c) Mass Spectrometry Conditions: ion gun is electric spray ion source (EI), and ion source temperature is 220 ~ 240 DEG C; Electron energy is 70ev; Mass range is 35-400m/z;
D () measures: adopt gas chromatography mass spectrometry to measure; Draw need testing solution, injection gas chromatography-GC-MS, measure, record 70min chromatogram, obtains finger-print.
2. the method for claim 1, is characterized in that: in the preparation of need testing solution, gets oral mushroom liquor 2 ~ 5L, and extract 2 ~ 4h with volatile oil extractor, obtain need testing solution, preferred extraction time is 3h.
3. the method for claim 1, is characterized in that: chromatographic column is fused-silica capillary column, and crosslinked 5% methyl-polysiloxane is Stationary liquid.
4. the method for claim 1, is characterized in that: preferred chromatographic column temperature programme condition is: initial temperature 50 DEG C (keeping 7min), is warming up to 70 DEG C (keeping 10min), then is warming up to 200 DEG C with 2.5 DEG C/min with 2.5 DEG C/min.
5. the method for claim 1, is characterized in that: vaporizer temperature 250 DEG C; Carrier gas is high-purity helium; Carrier gas flux 1.53mL/min; Split ratio 1:50.
6. the method for claim 1, is characterized in that: the accurate sample size drawing the need testing solution of inject gas chromatograph is 0.1 μ l.
7. the method for claim 1, is characterized in that: adopt gas chromatograph-mass spectrometer to measure; Draw need testing solution, injection gas chromatography-GC-MS, measure, record 70min chromatogram, identify the structure of the corresponding component in each peak according to library searching, and chromatographic peak area normalization method is calculated, ask for the percentage composition of each component, with No. 5 peak alpha-terpineols for reference peak, calculate relative retention time.
8. the method for claim 1, it is characterized in that: in the finger-print of described oral mushroom liquor, single peak area all exceedes total peak area 1% and determines that the total peak of composition has 8, the composition determined is as follows: No. 1 peak is cis-α, α-5-trimethyl-5-vinyl tetrahydrofuran-2-methyl alcohol, No. 2 peaks are trans linalool oxide, No. 3 peaks are linalool, No. 4 peaks are (R)-(-)-4-terpilenol, No. 5 peaks are alpha-terpineol, No. 6 peaks are geraniol, No. 7 peaks are inner mold-1, 3, 3-trimethyl two ring [2.2.1] heptane-2-alcohol acetic ester, No. 8 peaks are leukotrienes.
9. as claim 1 and method according to claim 7, it is characterized in that: the total peak that in the finger-print of described oral mushroom liquor, single peak area all exceedes total peak area 1% has 8, with No. 5 peak alpha-terpineols for reference peak, calculate relative retention time, the relative retention time at each peak is respectively: (1) 0.523 ~ 0.641, (2) 0.564 ~ 0.689, (3) 0.610 ~ 0.789, (4) 0.825 ~ 0.970, (5) 1.000, (6) 1.266 ~ 1.548, (7) 1.313 ~ 1.618, (8) 2.665 ~ 3.035; Preferred each peak relative retention time is respectively:, (1) 0.567 ~ 0.601, (2) 0.594 ~ 0.641, (3) 0.621 ~ 0.761, (4) 0.865 ~ 0.930, (5) 1.000, (6) 1.342 ~ 1.494, (7) 1.353 ~ 1.548, (8) 2.765 ~ 2.914.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105651725A (en) * | 2016-03-02 | 2016-06-08 | 广东太阳神集团有限公司 | Three-dimensional fingerprint spectrum of fruit bodies of hericium erinaceus and method for constructing three-dimensional fingerprint spectrum |
| CN109425677A (en) * | 2017-09-04 | 2019-03-05 | 天津中新药业研究中心 | A kind of method of quality control of inducing diaphoresis dampness elimination qi-regulating and middle drug |
| CN116570669A (en) * | 2023-04-18 | 2023-08-11 | 湖南汉森制药股份有限公司 | Method for treating diseases and Chinese medicinal composition used in same |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105651725A (en) * | 2016-03-02 | 2016-06-08 | 广东太阳神集团有限公司 | Three-dimensional fingerprint spectrum of fruit bodies of hericium erinaceus and method for constructing three-dimensional fingerprint spectrum |
| CN109425677A (en) * | 2017-09-04 | 2019-03-05 | 天津中新药业研究中心 | A kind of method of quality control of inducing diaphoresis dampness elimination qi-regulating and middle drug |
| CN109425677B (en) * | 2017-09-04 | 2021-08-10 | 天津中新药业研究院有限公司 | Quality control method for exterior syndrome relieving, dampness resolving, qi regulating and traditional Chinese medicine |
| CN116570669A (en) * | 2023-04-18 | 2023-08-11 | 湖南汉森制药股份有限公司 | Method for treating diseases and Chinese medicinal composition used in same |
| CN116570669B (en) * | 2023-04-18 | 2024-02-27 | 湖南汉森制药股份有限公司 | Method for treating diseases and Chinese medicinal composition used in same |
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Application publication date: 20160203 |