CN107727754B - HP L C fingerprint detection method of Xiaojin preparation - Google Patents
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Abstract
The invention discloses a traditional Chinese medicine fingerprint spectrum detection method of a Xiaojin preparation, which establishes liquid phase fingerprint spectrum measurement conditions and conducts methodology investigation by screening conditions such as instruments, chromatographic columns, mobile phases, detection wavelengths and the like, and establishes the fingerprint spectrum standard of the Xiaojin preparation according to a plurality of batches of mass production samples. Because the prescription of the product contains medicinal herbs such as plant medicines, animal medicines, resin and the like, the medicinal herbs have wide sources, a plurality of production areas, different quality and high quality standard limitations exist, in order to further improve the product quality and ensure the safe and effective medication, the Xiaojin preparation is controlled from the medicinal herbs resource, the product quality can be comprehensively and effectively controlled by adopting a fingerprint, a whole-process production quality control system is established, and a quality traceable system penetrating through a whole industrial chain is established on the basis.
Description
Technical Field
The invention belongs to the field of traditional Chinese medicine detection, and relates to an HP L C fingerprint detection method of Xiaojin preparation.
Background
The traditional Chinese medicine fingerprint is a traditional Chinese medicine quality control mode developed by using the common similarity of traditional Chinese medicine groups as a theoretical basis and by means of various technologies such as spectrum, chromatography and the like, the traditional Chinese medicine fingerprint is a spectrum which can mark common peaks of the characteristics of the traditional Chinese medicine after the traditional Chinese medicine is properly processed and is obtained by a certain analysis means, so that the authenticity of the traditional Chinese medicine is identified, the uniformity and the stability of the quality of the medicinal material are evaluated, the traditional Chinese medicine fingerprint can basically reflect the whole appearance of the traditional Chinese medicine within a certain range, the quality control index of the traditional Chinese medicine is upgraded from the original measurement of single component content to the detection of the internal quality of the whole traditional Chinese medicine, the comprehensive evaluation of the internal quality of the traditional Chinese medicine and the comprehensive control of the whole substances are realized, the quality of the traditional Chinese medicine is stable and controllable, the stability of the clinical curative effect of the traditional Chinese medicine is ensured, the traditional Chinese medicine research is more consistent with the holistic concept of the traditional Chinese medicine, the traditional Chinese medicine fingerprint detection methods such as a chromatographic method, a spectroscopic method, a spectral method, a spectroscopic method, a chromatography, a capillary electrophoresis, and the like, wherein the high performance liquid chromatography, the high performance, the ultraviolet detector, the.
A traditional Chinese medicine with the effects of dissipating stagnation, relieving swelling, removing blood stasis and relieving pain is collected from the first part of the 2010 edition of Chinese pharmacopoeia, and the medicine is named as Xiaojin pill and is prepared from 10 traditional Chinese medicines of artificial musk, semen momordicae, radix aconiti agrestis, resina liquidambaris, frankincense, myrrh, trogopterus dung, angelica sinensis, earthworm, fragrant ink and the like. The formula is a classic and famous traditional Chinese medicine formula, and can be used for treating various difficult and complicated diseases such as goiter, benign prostatic hyperplasia, postherpetic neuralgia, cystic hyperplasia of breast, chronic pelvic inflammatory disease mass, nodular fasciitis and the like. At present, various dosage forms such as tablets, capsules and the like are on the market, for example, CN106265992A discloses Xiaojin capsules and a preparation method thereof, and CN102764311A discloses Xiaojin dispersible tablets and a preparation method thereof. The existing Xiaojin preparation mainly adopts the mode of adding crude drug powder into the preparation.
The Xiaojin preparation contains medicinal sources such as plant medicines, animal medicines, resin and the like, has wide medicinal material sources, a plurality of production areas, different quality and high quality standard limitation, is intended to control the Xiaojin preparation from medicinal material base sources in order to further improve the product quality and ensure the safe and effective medication, adopts a fingerprint technology to comprehensively and effectively control the product quality, establishes a whole-process production quality control system, and establishes a quality traceable system penetrating through a whole industrial chain on the basis.
Disclosure of Invention
Aiming at the problem that the quality of a traditional Chinese medicine compound cannot be comprehensively controlled by the existing quality detection method of a Xiaojin preparation, the invention aims to establish an HP L C fingerprint detection method of the Xiaojin preparation.
In order to achieve the purpose, the invention adopts the following technical scheme:
the HP L C fingerprint detection method of Xiaojin preparation comprises the following raw materials, by weight, 1-20 parts of artificial musk, 40-60 parts of radix aconiti agrestis, 20-40 parts of frankincense, 40-60 parts of trogopterus dung, 40-60 parts of earthworm, 40-60 parts of momordica cochinchinensis seed, 40-60 parts of liquidambar formosana, 20-40 parts of myrrh, 20-40 parts of angelica sinensis and 1-10 parts of Chinese ink, and the detection method comprises the following steps:
(1) preparation of a test solution: grinding the preparation of the small gold to be detected, taking 0.5-5 parts by weight, adding 10-100 parts by volume of water-saturated n-butanol, weighing, refluxing, extracting, cooling to room temperature, weighing again, supplementing the lost weight with water-saturated n-butanol, shaking up, filtering with a microporous filter membrane, and taking the subsequent filtrate for later use;
(2) precisely absorbing 5-20 mu l of test solution, and detecting by using a high performance liquid chromatograph, wherein the high performance liquid chromatograph comprises an ultraviolet detector, the set detection wavelength of the ultraviolet detector is 200-300nm, and the stationary phase of the high performance liquid chromatograph is C18The chromatographic column adopts mixed solution of methanol and 0.05-0.2 wt% phosphoric acid solution as mobile phase and adopts gradientEluting at a flow rate of 0.5-2ml/min, at a column temperature of 25-40 deg.C, with theoretical plate number not less than 10000;
(3) recording a chromatogram of the test solution for 0-120min, respectively carrying out data import, multi-point correction and data matching on the chromatogram of the test solution by using a Chinese medicine chromatogram fingerprint similarity evaluation system of the State pharmacopoeia Committee to obtain a fingerprint and carrying out similarity analysis,
the relationship between the parts by weight and the parts by volume is g/m L.
Preferably, the set detection wavelength of the ultraviolet detector is 254 nm.
Preferably, the phosphoric acid solution has a weight concentration of 0.1%.
Preferably, in the gradient elution, the volume ratio of each time period and the 0.1% phosphoric acid solution phase in the mobile phase is: 0-2 min, and 70% of phosphoric acid solution phase; 2-20 min, and 70-45% of phosphoric acid solution phase; 20-50 min, and 45-25% of phosphoric acid solution phase; 50-70 min, 25-20% of phosphoric acid solution phase; 70-85 min, and 20-15% of phosphoric acid solution phase; 85-90 min, and 15-5% of phosphoric acid solution phase; 90-120 min, 5-0% of phosphoric acid solution phase.
Preferably, the chromatogram of the test solution has 20 common characteristic peaks, wherein the peak 1 is a specific peak of artificial musk, the peak 4 is a specific peak of sweetgum resin, the peaks 8 and 14 are specific peaks of frankincense, the peak 9 is a specific peak of trogopterus dung, the peaks 15 and 18 are specific peaks of myrrh, the common peak 13 of sweetgum resin and myrrh is taken as a reference peak, the relative retention time of each peak is 5.997min for the peak 1, 18.900min for the peak 4, 38.318min for the peak 8, 45.058min for the peak 9, 59.838min for the peak 13, 69.005min for the peak 14, 76.934min for the peak 15, and 90.353min for the peak 18.
The concentrations of the phosphoric acid solution to be referred to in the present invention are volume concentrations, and for example, 0.1% phosphoric acid solution means that 0.1ml of phosphoric acid is contained per 100ml of phosphoric acid aqueous solution.
The invention has the beneficial effects that:
the method comprises the steps of establishing HP L C fingerprint of the Xiaojin preparation, measuring 10 batches of Xiaojin capsules, marking out 20 common peaks and a standard fingerprint, obtaining the chromatogram with similarity of more than 0.97, calculating the stability, the stability and the repeatability by using the relative retention time and the relative peak area, wherein the RSD value of the relative retention time is less than 2.0%, the RSD value of the relative peak area is less than 5.0%, and identifying the specific peak area of the musk in 20 artificial balsam, 5 g.
The fingerprint spectrum of the Xiaojin preparation established by the invention can be used for controlling the basic source of the raw medicinal materials, can effectively guide the feeding in the production process and strictly standardize the production operation, really ensures the safety, effectiveness and reliability of clinical medication, and has the advantages of convenient and rapid operation and the like compared with other detection methods.
Drawings
FIG. 1 is a HP L C map of a sample to be tested after methanol ultrasonic extraction.
FIG. 2 is a HP L C map of a sample to be tested after reflux extraction of water-saturated n-butanol.
FIG. 3 is a HP L C spectrum obtained at a detection wavelength of 210 nm.
FIG. 4 is a spectrum of HP L C at a detection wavelength of 254 nm.
FIG. 5 is a spectrum of HP L C at a detection wavelength of 267 nm.
FIG. 6 is a HP L C spectrum obtained at a detection wavelength of 280 nm.
FIG. 7 is a HP L C spectrum obtained at a detection wavelength of 300 nm.
Fig. 8 is HP L C standard fingerprint of xiaojin capsule.
Figure 9 is the HP L C standard fingerprint of musk in the formula of xiaojin capsules.
FIG. 10 shows the HP L C standard fingerprint of Boswellia carterii in the prescription of Xiaojin capsule.
FIG. 11 is the HP L C standard fingerprint of Myrrha in the recipe of Xiaojin Capsule.
FIG. 12 is the HP L C standard fingerprint of Liquidambar formosana Hance in Xiaojin Capsule prescription.
FIG. 13 is the HP L C standard fingerprint of Oletum Trogopterori in the prescription of Xiaojin capsule.
FIG. 14 shows the HP L C standard fingerprint of Angelica sinensis in Xiaojin capsule prescription.
Detailed Description
The present invention will be described in detail below with reference to specific examples, which are given by way of illustration of the gold capsules.
The small gold capsules used in the following examples were provided by the health care pharmaceutical group, ltd. 30g of artificial musk, 150g of semen momordicae, 150g of radix aconiti agrestis, 150g of resina liquidambaris, 75g of frankincense, 75g of myrrh, 150g of trogopterus dung, 75g of angelica, 150g of earthworm and 12g of Chinese ink, and the raw materials are crushed and filled into capsules.
1. Instrument and reagent
A Waters e2695 high performance liquid chromatograph, a quaternary pump, an online vacuum degassing system, an automatic sample injector, a column incubator and an ultraviolet detector; AB204-E electronic balance (Shanghai Merle-Torledo instruments, Inc.).
10 batches of small gold capsules (170116 + 0121, 170332 + 0335, 10 batches); methanol is chromatographic grade, and water is purified water.
2. Method step
(1) Preparing a test solution: grinding the content of the small gold capsules, precisely weighing 1g of the small gold capsules, precisely adding 50ml of water-saturated n-butanol, weighing, performing reflux extraction, cooling to room temperature, weighing again, supplementing the loss weight with the water-saturated n-butanol, shaking up, filtering with a microporous filter membrane, and taking the subsequent filtrate for later use;
(2) chromatographic conditions are as follows: agilent ZORBAX SB C184.6 × 250mm, 5 μm, and the mobile phase is methanol-0.1% phosphorus solution as the mobile phase, and the gradient elution is performed, wherein the phase A is methanol, the phase B is 0.1% phosphoric acid solution, and the phase B is 70% in 0-2 min;2-20 min, and 70-45% of phase B; 20-50 min, 45-25% of phase B; 50-70 min, 25-20% of phase B; 70-85 min, 20-15% of phase B; 85-90 min, 15-5% of phase B; 90-120 min, 5-0% of phase B; flow rate: 1 ml/min; the detection wavelength is 254 nm; the column temperature is 35 ℃; the amount of the sample was 10. mu.l. The number of theoretical plates is not less than 10000 calculated according to No. 13 peak.
(3) Methodology investigation: performing precision test, stability test and repeatability test according to the requirement of the fingerprint;
(4) and (3) sample determination: taking several batches of Xiaojin capsules, respectively preparing 10 parts of test solution according to the method in the step (1), precisely sucking 10 mu l of each test solution, determining by adopting the chromatographic conditions in the step (2), recording a chromatogram of 0-120min, and calculating relative retention time and relative peak area by taking a No. 13 peak as a reference peak in the chromatogram;
(5) establishing a fingerprint and analyzing peak attribution: taking several batches of small gold capsule samples respectively, preparing a test solution according to the step (1), determining according to the chromatographic conditions of the step (2), recording a chromatogram for 120min, concentrating all chromatographic peaks within 120min, comparing the chromatograms of the batches of samples, determining 20 common peaks, and performing fingerprint spectrum research on each medicinal material in the prescription under the condition of the finished product chromatographic fingerprint spectrum, and performing peak attribution analysis; by comparing with the raw material medicine atlas in the prescription, the 1 st peak is the peculiar peak of artificial musk, the 4 th peak is the peculiar peak of sweetgum resin, the 8 th and 14 th peaks are the peculiar peak of frankincense, the 9 th peak is the peculiar peak of trogopterus dung, and the 15 th and 18 th peaks are the peculiar peak of myrrh. The common peak 13 of the resina Liquidambaris and the prepared myrrh is selected as a reference peak, the relative retention time of each peak is respectively 5.997min for the peak 1, 18.900min for the peak 4, 38.318min for the peak 8, 45.058min for the peak 9, 59.838min for the peak 13, 69.005min for the peak 14, 76.934min for the peak 15 and 90.353min for the peak 18.
(6) Calculating the similarity of the samples: and introducing the 10 batches of the minigold capsule chromatograms into a 2004 edition of a Chinese medicine chromatogram fingerprint similarity evaluation system issued by the State pharmacopoeia Committee, selecting a time window with the width of 0.1min, generating a comparison spectrum by adopting a sample 1, generating a chromatogram fingerprint common mode through multipoint correction and data matching, and carrying out similarity analysis on the fingerprints of the 10 batches of samples.
3. Preparing a test solution: according to the raw material components of the Xiaojin capsule, petroleum ether, methanol, 95% ethanol and water-saturated n-butyl alcohol are respectively considered as extraction solvents, and through comprehensive analysis, a test solution obtained by extracting the water-saturated n-butyl alcohol can comprehensively reflect main components in a finished product and has good repeatability, so that the water-saturated n-butyl alcohol is determined as the extraction solvent; and the extraction method (ultrasonic and reflux) is examined, the fingerprint base line of the sample extracted by reflux is found to be more stable than that of ultrasonic extraction, and finally the preparation method for determining the sample by the preparation fingerprint is determined as follows: grinding XIAOJIN Capsule, collecting about 1g, precisely weighing, precisely adding water saturated n-butanol 50ml, weighing, reflux extracting, cooling to room temperature, weighing, supplementing water saturated n-butanol to reduced weight, shaking, filtering with microporous membrane, and collecting the filtrate. The partial fingerprint is shown in figure 1-2.
4. Establishment of detection method
4.1 instruments, reagents and chromatographic conditions
The instrument comprises the following steps: a Waters e2695 high performance liquid chromatograph, a quaternary pump, an online vacuum degassing system, an automatic sample injector, a column temperature box,
reagent: the methanol is chromatographically pure, the n-butanol is analytically pure, and the water is purified water.
A chromatographic column: agilent ZORBAX SB-C184.6 × 250mm, 5 μm, detection wavelength of 210, 254, 267, 280, 300nm, sample volume of 10 μ l, column temperature of 30-40 ℃ and flow rate of 1 ml/min.
4.2 selection of the Mobile phase
Through comparison and screening, the methanol- (B)0.1 percent phosphoric acid solution system (A) is eluted by linear gradient, and the obtained liquid chromatogram has more stable base line, more symmetrical chromatographic peak shape and better separation degree.
4.3 optimization of gradient elution procedure: through systematic exploration and optimization, the following linear gradient elution procedures are found to be capable of comprehensively detecting chemical components in the preparation and also capable of enabling the components to obtain ideal separation effects: 0-2 min, 70% of phase B; 2-20 min, and 70-45% of phase B; 20-50 min, 45-25% of phase B; 50-70 min, 25-20% of phase B; 70-85 min, 20-15% of phase B; 85-90 min, 15-5% of phase B; 90-120 min, 5-0% of phase B; i.e. 1 sample analysis procedure was completed. The recording time is 0-120 min.
4.4 determination of optimal measurement wavelength: through comparative analysis of liquid chromatogram maps, the base line of the preparation maps at 210nm, 267nm, 280nm and 300nm is relatively flat, the peak shapes are not wrong, but the peaks are few, and the components of the preparation cannot be comprehensively reflected; under 254nm, the separation degree of fingerprint peaks of each component is good, the number of chromatographic peaks, a base line and the signal response strength are comprehensively considered, and 254nm is determined as the optimal detection wavelength of the fingerprint. The fingerprint is shown in fig. 3-7.
5. Methodology investigation
5.1 stability test: taking the sample solution, measuring at 0, 4, 8 and 12h according to the conditions of the chromatographic terms, and observing the relative retention time of each common peak and the RSD of the relative peak area. The results show that the relative retention time of each spectrum peak is less than 1.0 percent, the relative peak area of each spectrum peak is less than 3.0 percent, and the fingerprint spectrum technical requirements are met. See tables 1-2.
Table 1 stability study relative retention time
Table 2 stability investigation relative peak area
5.2 repeatability test: taking 6 parts of samples of the same batch, preparing 6 parts of test solution according to the test solution preparation method under item 1, measuring under the chromatographic conditions, and observing the relative retention time of each common peak and the RSD of the relative peak area. The results show that the relative retention time of each spectrum peak is less than 1.0 percent, the relative peak area of each spectrum peak is less than 4.0 percent, and the fingerprint spectrum technical requirements are met. See tables 3-4.
TABLE 3 repeated examination of relative retention time
TABLE 4 relative peak area for repeated examination
5.3 precision test: and taking a sample solution to be tested, continuously injecting samples for 6 times according to the conditions under the chromatographic terms, and inspecting the relative retention time of each common peak and the RSD of the relative peak area. The results show that the relative retention time of each spectrum peak is less than 1.0 percent, the relative peak area of each spectrum peak is less than 4.0 percent, and the fingerprint spectrum technical requirements are met. See tables 5-6.
TABLE 5 relative retention time with precision
TABLE 6 relative peak area for precision investigation
6. Establishing a fingerprint spectrum: 10 batches of small gold capsule samples are respectively taken to prepare a test solution, a chromatogram in 125min is measured and recorded, and as a result, all chromatographic peaks are concentrated in 125min, the chromatograms of the 10 batches of samples are compared, and 20 common peaks are determined. Confirming that the 13 # peak with the retention time of 59.838min is selected as a reference peak;
6.1 sample similarity calculation: introducing 10 batches of the Xiaojin capsule chromatograms into a traditional Chinese medicine chromatogram fingerprint similarity evaluation system (2004 edition) issued by the State pharmacopoeia Committee, selecting a time window with the width of 0.1min, generating a comparison spectrum by adopting a sample 1, generating a chromatogram fingerprint common mode through multipoint correction and data matching, and obtaining the 10 batches of sample fingerprint similarity calculation results shown in a table 7.
TABLE 7 similarity of ten samples
| Batch number | Degree of similarity |
| 170116 | 0.987 |
| 170117 | 0.994 |
| 170118 | 0.983 |
| 170119 | 0.993 |
| 170120 | 0.994 |
| 170121 | 0.981 |
| 170332 | 0.996 |
| 170333 | 0.991 |
| 170334 | 0.977 |
| 170335 | 0.981 |
| Comparison fingerprint | 1 |
6.2 Standard fingerprint of Xiaojin Capsule
Taking a plurality of batches of Xiaojin capsules, respectively preparing a sample solution according to the preparation method of the sample solution, establishing a high performance liquid chromatogram of the Xiaojin capsule preparation according to a plurality of batches of detection data obtained by detection, determining the peak retention time and the peak area value of the high performance liquid chromatogram, then collecting all detection data, calculating the average value of the relative retention time of each corresponding peak, the average value and the standard deviation of the relative peak area, and the like, respectively dividing the average retention time and the average peak area of a reference peak, and taking the average retention time and the relative peak area value of a standard fingerprint, deriving a calculation result, making standard fingerprint data, drawing the standard fingerprint, wherein the standard fingerprint is shown in a figure 8, and the result is shown in a table 8.
TABLE 8 Standard fingerprint data
6.3 correlation between the fingerprints of the herbs and the finished products
Preparing a medicinal material test solution: the raw materials in the prescription are respectively taken and prepared into capsules according to a Xiaojin capsule preparation process, and chromatographic peak assignment is carried out according to standard fingerprint spectrum conditions. The finger prints are shown in FIGS. 9-14, and the results are shown in Table 9.
TABLE 9 correlation atlas of Xiaojin capsules and herbs
Claims (1)
1. The HP L C fingerprint detection method of Xiaojin preparation is characterized in that the Xiaojin preparation is prepared from the following raw materials, by weight, 1-20 parts of artificial musk, 40-60 parts of kusnezoff monkshood root, 20-40 parts of frankincense, 40-60 parts of trogopterus dung, 40-60 parts of earthworm, 40-60 parts of cochinchina momordica seed, 40-60 parts of liquidambar formosana, 20-40 parts of myrrh, 20-40 parts of Chinese angelica and 1-10 parts of Chinese ink, and the detection method comprises the following steps:
(1) preparation of a test solution: grinding the preparation of the small gold to be detected, taking 0.5-5 parts by weight, adding 10-100 parts by volume of water-saturated n-butanol, weighing, refluxing, extracting, cooling to room temperature, weighing again, supplementing the lost weight with water-saturated n-butanol, shaking up, filtering with a microporous filter membrane, and taking the subsequent filtrate for later use;
(2) precisely absorbing 5-20 μ l of sample solution, and detecting with High Performance Liquid Chromatograph (HPLC) having ultraviolet detector with set detection wavelength of 254nm, and stationary phase of HPLC being C18A chromatographic column, wherein the mobile phase is a mixed solution of methanol and 0.1% phosphoric acid solution, gradient elution is adopted, the flow rate is 0.5-2ml/min, the column temperature is 25-40 ℃, and the number of theoretical plates is not less than 10000;
in the gradient elution, the volume ratio of each time period and the 0.1% phosphoric acid solution phase in the mobile phase is respectively as follows: 0-2 min, and 70% of phosphoric acid solution phase; 2-20 min, 70 → 45% of phosphoric acid solution phase; 20-50 min, 45 → 25% of phosphoric acid solution phase; 50-70 min, 25 → 20% of phosphoric acid solution phase; 70-85 min, 20 → 15% of phosphoric acid solution phase; 85-90 min, 15 → 5% of phosphoric acid solution phase; 90-120 min, 5 → 0% of phosphoric acid solution phase;
(3) recording a chromatogram of the test solution for 0-120min, respectively carrying out data import, multi-point correction and data matching on the chromatogram of the test solution by using a Chinese medicine chromatogram fingerprint similarity evaluation system of the State pharmacopoeia Committee to obtain a fingerprint and carrying out similarity analysis,
the relation between the parts by weight and the parts by volume is g/m L,
the chromatogram of the test solution has 20 common characteristic peaks, wherein the peak 1 is a specific peak of artificial musk, the peak 4 is a specific peak of sweetgum resin, the peaks 8 and 14 are specific peaks of frankincense, the peak 9 is a specific peak of trogopterus dung, the peaks 15 and 18 are specific peaks of myrrh, the common peak 13 of sweetgum resin and myrrh is taken as a reference peak, the relative retention time of each peak is 5.997min for the peak 1, 18.900min for the peak 4, 38.318min for the peak 8, 45.058min for the peak 9, 59.838min for the peak 13, 69.005min for the peak 14, 76.934min for the peak 15, and 90.353min for the peak 18.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104739956A (en) * | 2015-02-27 | 2015-07-01 | 武汉健民药业集团股份有限公司 | Use of traditional Chinese medicine composition in preparing antiandrogen drug |
-
2017
- 2017-09-01 CN CN201710780630.9A patent/CN107727754B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104739956A (en) * | 2015-02-27 | 2015-07-01 | 武汉健民药业集团股份有限公司 | Use of traditional Chinese medicine composition in preparing antiandrogen drug |
Non-Patent Citations (4)
| Title |
|---|
| HＰLＣ-Ｑ-ＴＯＦ-MＳ 法测定不同厂家小金丸中9 种乌头类生物碱的含量;黄阳 等;《海峡药学》;20161231;第28卷(第9期);1-5 * |
| HPLC测定小金胶囊中乌头碱的含量;侯亚会 等;《成都中医药大学学报》;20090630;第32卷(第2期);摘要，第90页 * |
| 超高效液相色谱质谱联用技术同时测定小金丸中7种成分的含量;蔡博 等;《中国药学杂志》;20151231;第50卷(第8期);第719页，第721页 * |
| 高效液相色谱法测定小金丸软胶囊中阿魏酸的含量;王欣 等;《中国医院药学杂志》;20071231;第27卷(第3期);全文 * |
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