CN105784951A - Multiple indicator rapid detection method for raw medicinal powder of condensed pill of six drugs with rehmannia - Google Patents
Multiple indicator rapid detection method for raw medicinal powder of condensed pill of six drugs with rehmannia Download PDFInfo
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Abstract
The invention relates to a multiple indicator rapid detection method for a raw medicinal powder of a condensed pill of six drugs with rehmannia. The method comprises the steps of: (1) acquiring raw powders of different batches; (2) determining the content of loganin using HPLC, determining water content by a drying method, and determining an extract content by using a cold soak method; (3) collecting near infrared spectrum data of key detection indicators for the raw medicinal powder of condensed pill of six drugs with rehmannia; (4) modeling near-infrared spectrum and preprocessing band spectrum; (5) establishing a rapid detection and correction model of contents of water, extract and loganin in the raw medicinal powder of the condensed pill of six drugs with rehmannia; and (6) using the correction model for the rapid determination of contents of water, extract and loganin in the raw medicinal powder of the condensed pill of six drugs with rehmannia. The present invention introduces the near infrared spectrum technology; and compared with traditional method, the established analytical method can quickly determine whether the quality of raw medicinal powder is qualified and determine whether the raw medicinal powder can enter the subsequent production process, so as to meet the requirements of fast and efficient production.
Description
Technical field
The invention belongs near infrared detection field, be specifically related to the method for quick of a kind of LIUWEI DIHUANG WAN concentrated pill crude drug powder.
Background technology
LIUWEI DIHUANG WAN concentrated pill records in " Chinese Pharmacopoeia " 2010 editions one, the powder that its crude drug powder is Cornaceae plant Fructus Corni CornusoffficinalisSieb.etZucc. drying and ripening sarcocarp and Dioscoreaceae plant Rhizoma Dioscoreae DioscoreaoppositaThumb. dry rhizome is mixed to get with 2:3 ratio.Recording LIUWEI DIHUANG WAN concentrated pill in 2010 editions " Chinese Pharmacopoeia " and have effect of enriching yin and nourishing kidney, for damage of kidney-YIN, dizziness and tinnitus, soreness of the waist and knees, osteopyrexia and fever, night sweat is passed out semen, and quenches one's thirst.Owing to LIUWEI DIHUANG WAN concentrated pill crude drug powder is the mixture of Fructus Corni and Rhizoma Dioscoreae, its chemical composition is extremely complex, mainly includes polysaccharide, organic acid, iridoid, dioscin etc..Fructus Corni and the pharmacological action of Rhizoma Dioscoreae, chemical composition have been carried out big quantity research by recent domestic scholar, the crude drug that LIUWEI DIHUANG WAN concentrated pill crude drug powder is important in producing as LIUWEI DIHUANG WAN concentrated pill, need to set up quality evaluation index, ensure quality and effect of preparation.But traditional detection method is time-consuming, effort, it is difficult to is widely used in production practices, therefore develops a kind of method that can quickly detect LIUWEI DIHUANG WAN concentrated pill crude drug opaque amount, the control comprehensively being used for on-the-spot medical material screening and quality has necessity and development prospect.
Near infrared spectrum (NIR) technology is a kind of indirect analysis technology, is that the foundation by calibration model realizes the qualitative or quantitative analysis to unknown sample, has quick, lossless, original position and the feature such as pollution-free.In recent years, near-infrared spectrum technique is as a kind of indirect analysis technology, it is applied in Chinese medicine quality control and production application field, including the qualitative, quantitative of the various dosage form of medical material, herbal mixture and Chinese medicine, and has utilized fibre-optical probe technology to realize the on-line continuous monitoring etc. to Chinese medicine production technology.Near-infrared spectrum technique is applied to the quick detection of LIUWEI DIHUANG WAN concentrated pill crude drug powder, its quality is controlled from the source that LIUWEI DIHUANG WAN concentrated pill produces, thus ensureing the safety of end product quality, stability and effectiveness, reach purpose fast and efficiently.
Summary of the invention
Present invention aim at providing a kind of LIUWEI DIHUANG WAN concentrated pill crude drug powder multiple index quick detecting method.Near-infrared spectrum technique is adopted can quickly to measure the content of moisture, extract content and loganin in LIUWEI DIHUANG WAN concentrated pill crude drug powder, it is achieved the Fast Evaluation of LIUWEI DIHUANG WAN concentrated pill crude drug opaque amount.
It is an object of the invention to be achieved through the following technical solutions:
(1) the LIUWEI DIHUANG WAN concentrated pill crude drug powder of different production batch is gathered
Gathering the LIUWEI DIHUANG WAN concentrated pill crude drug powder sample of different production batch, medical material after crushed, is crossed 80～120 mesh sieves, is obtained even-grained LIUWEI DIHUANG WAN concentrated pill crude drug powder powder.
(2) the crucial Testing index of LIUWEI DIHUANG WAN concentrated pill crude drug powder is measured
Choose moisture, extract content, Determination of Loganin as the crucial Testing index of LIUWEI DIHUANG WAN concentrated pill crude drug powder；Adopting moisture analysis content in " Chinese Pharmacopoeia ", adopt cold-maceration in " Chinese Pharmacopoeia " to measure extract content, LIUWEI DIHUANG WAN concentrated pill crude drug powder, after pretreatment, adopts high effective liquid chromatography for measuring Determination of Loganin.
(3) LIUWEI DIHUANG WAN concentrated pill crude drug powder calibration set sample and the near-infrared original spectral data of checking collection sample are gathered
Precision weighs LIUWEI DIHUANG WAN concentrated pill crude drug powder medicinal powder 1～5g, is placed in culture dish, keeps powder surface smooth, adopts diffuse-reflectance method to gather near infrared spectrum, and with air for reference, scanning times is 1-640 time, and resolution is 2-16cm-1, scanning optical spectrum ranges for 4000-12000cm-1。
(4) pretreatment of near-infrared original spectrum
The near-infrared original spectrum that step (3) gathers carries out pretreatment, with filter information, reduce noise, adopt first derivative, second dervative, multiplicative scatter correction, Norris to smooth, deduct the combination of 1 to 2 kind of method in straight line, SNV the spectrum eliminating spectral singularity value is carried out pretreatment, including:
1) LIUWEI DIHUANG WAN concentrated pill crude drug powder moisture model adopts and deducts straight line pretreatment；
2) LIUWEI DIHUANG WAN concentrated pill crude drug powder extract content model adopts and eliminates constant offset Pretreated spectra；
3) the Determination of Loganin model of LIUWEI DIHUANG WAN concentrated pill crude drug powder adopts vector quantization normalizing (SNV) Pretreated spectra.
(5) select the crucial Testing index modeling wave band of LIUWEI DIHUANG WAN concentrated pill crude drug powder, set up near infrared correction
By the near infrared spectrum of LIUWEI DIHUANG WAN concentrated pill crude drug powder calibration set sample after Pretreated spectra, its modeling waveband selection is as follows: water model modeling wave band is 9403.7-7498.3cm-1And 6102-4246.7cm-1；Extractum model modeling wave band is 7502.1-4597.7cm-1；Determination of Loganin model modeling wave band is 7502.1-4246.7cm-1, adopt partial least square method (PLS) to set up the quantitative calibration models between near infrared spectrum and above-mentioned each Testing index.
The calibration model set up adopts correlation coefficient (R), relation analysis error (RPD), four parameters of cross validation root-mean-square (RMSECV) number of principal components (Factor) investigate model performance, adopt prediction mean square deviation (RMSEP) simultaneously, relative deviation (RSEP) carrys out the evaluation model predictive ability to unknown sample, when R value is close to 1, when RPD value more than 2.5 and more big evaluation model performance more good, prediction accuracy is high, when RMSEP is more little, when RSEP value is less than 10%, evaluation model has good predictive ability, disclosure satisfy that the requirement that LIUWEI DIHUANG WAN concentrated pill crude drug powder quickly detects.
(6) checking of calibration model
With the checking collection sample described in step (3), the calibration model described in step (5) is verified, after adopting the preprocess method identical with step (4) described calibration set sample near-infrared original spectrum, steps for importing (5) described calibration model, the performance of checking calibration model.
(7) measure the near infrared spectrum data of LIUWEI DIHUANG WAN concentrated pill crude drug powder sample to be measured, steps for importing (5) described calibration model, calculate the prediction content obtaining moisture in testing sample, extractum, loganin through model.
High effective liquid chromatography for measuring Determination of Loganin method described in detection method step (2) of the present invention is: 1) preprocess method is: take LIUWEI DIHUANG WAN concentrated pill crude drug powder (crossing 80-120 mesh sieve) about 0.5-1g, accurately weighed, put in tool plug conical flask, precision adds 80% methanol of 30-100mL, it is heated to reflux 0.5-2h, it is re-weighed, supplies weightlessness with 80% methanol；Extracting solution is centrifuged 10min, and rotating speed is 10000-15000r min-1, take supernatant, both；2) liquid phase chromatogram condition: chromatographic column: WatersCORTECSC18 analytical column (4.6 × 150mm, 2.7 μm)；Mobile phase is acetonitrile (B): water (A), gradient elution 0～10min:10～17%B, 10～15min:17～90%B；Detection wavelength 220-260nm, flow velocity is 0.8-1mL min-1, sample size is 5-25 μ L, column temperature 25-35 DEG C.
Above-mentioned high effective liquid chromatography for measuring Determination of Loganin method is preferably: 1) preprocess method is: take LIUWEI DIHUANG WAN concentrated pill crude drug powder (crossing 100 mesh sieves) about 0.5g, accurately weighed, put in tool plug conical flask, precision adds 80% methanol of 50mL, it is heated to reflux 1h, it is re-weighed, supplies weightlessness with 80% methanol；Extracting solution is centrifugal 10min to the centrifuge tube of 1.5mL, and rotating speed is 13000r min-1, take supernatant, both；2) liquid phase chromatogram condition: chromatographic column: WatersCORTECSC18 analytical column (4.6 × 150mm, 2.7 μm)；Mobile phase is acetonitrile (B): water (A), gradient elution 0～10min:10～17%B, 10～15min:17～90%B；Detection wavelength 240nm, flow velocity is 0.8mL min-1, sample size is 10 μ L, column temperature 30 DEG C.
Gathering near infrared light time spectrum in detection method step (3) of the present invention, described scanning times is preferably 32 times, and resolution is preferably 8cm-1。
LIUWEI DIHUANG WAN concentrated pill crude drug powder multiple index quick detecting method of the present invention is used to measure the prediction content of the crucial Testing index in LIUWEI DIHUANG WAN concentrated pill crude drug powder, moisture≤16.0%, extract content >=24.0%, Determination of Loganin >=0.24% in the prediction content of the crucial Testing index of the LIUWEI DIHUANG WAN concentrated pill crude drug powder to be measured recorded, then judge that this LIUWEI DIHUANG WAN concentrated pill crude drug powder is qualified samples, conform to quality requirements, it is possible to put into the subsequent production links such as extraction.
NIR technology is incorporated in the detection of LIUWEI DIHUANG WAN concentrated pill crude drug powder by the present invention, realize the quick mensuration to each Testing index (moisture, extractum, Determination of Loganin), from source, raw-material quality is controlled in Chinese medicine produces, shorten the detection time, save production cost, improve production efficiency and economic benefit, fully ensure that LIUWEI DIHUANG WAN concentrated pill constant product quality, reliable.
Accompanying drawing explanation
Accompanying drawing 1 is LIUWEI DIHUANG WAN concentrated pill crude drug powder powder near-infrared original absorbance spectrogram
Accompanying drawing 2 is the relevant figure of LIUWEI DIHUANG WAN concentrated pill crude drug powder aqueous powder content measured value and near-infrared predictive value
Accompanying drawing 3 is the relevant figure of LIUWEI DIHUANG WAN concentrated pill crude drug powder powder extract content measured value and near-infrared predictive value
Accompanying drawing 4 is the relevant figure of LIUWEI DIHUANG WAN concentrated pill crude drug powder powder Determination of Loganin measured value and near-infrared predictive value
Accompanying drawing 5 is the comparison diagram of LIUWEI DIHUANG WAN concentrated pill crude drug powder aqueous powder measured value and near-infrared predictive value
Accompanying drawing 6 is the comparison diagram of LIUWEI DIHUANG WAN concentrated pill crude drug powder powder extractum measured value and near-infrared predictive value
Accompanying drawing 7 is the comparison diagram of LIUWEI DIHUANG WAN concentrated pill crude drug powder powder Determination of Loganin measured value and near-infrared predictive value
Detailed description of the invention
The present invention is further described in conjunction with the accompanying drawings and embodiments.
Embodiment 1:
(1) the LIUWEI DIHUANG WAN concentrated pill crude drug powder of different production batch is gathered
By the LIUWEI DIHUANG WAN concentrated pill crude drug powder of different production batch after crushed, cross 100 mesh sieves, obtain granularity more uniform LIUWEI DIHUANG WAN concentrated pill crude drug powder powder.
(2) mensuration of LIUWEI DIHUANG WAN concentrated pill crude drug powder key Testing index
1. determination of water method: the official weighting method after dried of determination of water of LIUWEI DIHUANG WAN concentrated pill crude drug powder, takes and dries the flat bottle (X to constant weight (double difference of weighing is less than 5mg)0), take 2g LIUWEI DIHUANG WAN concentrated pill crude drug powder medical material, precise weighing (X1), put 105 DEG C of baking 5h in vacuum drying oven, take out and put cooling 30min in exsiccator, weigh, then put baking 1h in vacuum drying oven, weigh (X2), the above person of weight differential 5mg continues to put baking in baking oven, until difference is less than 5mg.Weight according to less loss, calculates water content (%) in test sample.
Moisture (%)=(X1-X2+X0)/X1×100。
2. determination of extractives method: taking about 2g LIUWEI DIHUANG WAN concentrated pill crude drug powder, put in 250mL conical flask, add water 50mL, close plug, merceration weighed quality.Front 6h jolting constantly, then stand 18h, weighed quality, by the quality of water deficiency less loss, shake up.Being placed in 15mL centrifuge tube and be centrifuged 30min, rotating speed is 3800r/min, and precision measures supernatant 10mL, puts and is dried to (X in the flat bottle of constant weight0), after water-bath is evaporated, in 105 DEG C of dry 3h, put cooling 30min, rapid accurately weighed weight (X in exsiccator2).The content (%) of extractum in test sample is calculated with dry product.
Content (%)=(X of extractum2-X0)×5/X1×100。
3. Determination of Loganin adopts high-performance liquid chromatogram determination: a. preprocess method is: take LIUWEI DIHUANG WAN concentrated pill crude drug powder (crossing 100 mesh sieves) about 0.5g, accurately weighed, put in tool plug conical flask, precision adds 80% methanol of 50mL, it is heated to reflux 1h, it is re-weighed, supplies weightlessness with 80% methanol.Extracting solution is centrifugal 10min to the centrifuge tube of 1.5mL, and rotating speed is 13000r min-1, take supernatant, both.B. liquid phase chromatogram condition: chromatographic column: WatersCORTECSC18 analytical column (4.6 × 150mm, 2.7 μm)；Mobile phase is acetonitrile (B): water (A), gradient elution 0～10min:10～17%B, 10～15min:17～90%B；Detection wavelength 240nm, flow velocity is 0.8mL min-1, sample size is 10 μ L, column temperature 30 DEG C.
(3) the near-infrared original spectral data of LIUWEI DIHUANG WAN concentrated pill crude drug powder calibration set sample and checking collection sample gathers
Precision weighs LIUWEI DIHUANG WAN concentrated pill crude drug powder powder 2g, is placed in weighing botle, keeps powder surface smooth, adopts diffuse-reflectance method to gather near infrared spectrum, and with air for reference, scanning times is 32, and resolution is 8cm-1, scanning optical spectrum ranges for 4000-10000cm-1, every batch sample scanning multiple scanning 4 times, it is averaged spectrum.LIUWEI DIHUANG WAN concentrated pill crude drug powder powder near-infrared original absorbance spectrogram is shown in accompanying drawing 1.
(4) pretreatment of near-infrared original spectrum
Offset minimum binary (PLS) method is used to set up the Near-Infrared Quantitative Analysis model of 3 Testing index in sample.Calibration set spectrum is carried out abnormity point differentiation before setting up by model, to improve model accuracy, original spectrum eliminates instrumental background or the drift impact on signal under the suitable preprocessing procedures such as smooth, differential simultaneously, suitable wave band is selected to extract effective information, reduce amount of calculation, shorten the modeling time.LIUWEI DIHUANG WAN concentrated pill crude drug powder original spectrum adopts a large amount of pretreatment modes that OPUS software provides, and smooths including first derivative, second dervative, multiplicative scatter correction, Norris, deducts in straight line, SNV the methods such as the combination of 1 to 2 kind of method spectral effective information is extracted.According to model parameter parameter, the Pretreated spectra mode of final each crucial Testing index is as follows:
1) LIUWEI DIHUANG WAN concentrated pill crude drug powder moisture model adopts and deducts straight line Pretreated spectra；
2) LIUWEI DIHUANG WAN concentrated pill crude drug powder extract content model adopts and eliminates constant offset Pretreated spectra；
3) the Determination of Loganin model of LIUWEI DIHUANG WAN concentrated pill crude drug powder adopts the Pretreated spectra of vector quantization normalizing (SNV)；(5) select each Testing index modeling wave band of LIUWEI DIHUANG WAN concentrated pill crude drug powder, set up near infrared correction
The near infrared spectrum of LIUWEI DIHUANG WAN concentrated pill crude drug powder medical material is after Pretreated spectra, and it models waveband selection: water model modeling wave band is 9403.7-7498.3cm-1And 6102-4246.7cm-1；Extractum model modeling wave band is 7502.1-4597.7cm-1；Determination of Loganin model modeling wave band is 7502.1-4246.7cm-1.The near infrared light spectrum information of gained is associated by Applied Chemometrics software with the standard value measured by reference method, adopts offset minimum binary (PLS) method to set up the quantitative calibration models between near infrared spectrum and above-mentioned each Testing index；
In modeling process, randomly choosing the sample of about 2/3rds as calibration set, remaining sample is used for predicting as checking collection.Model adopts correlation coefficient (R), relation analysis error (RPD), cross validation root-mean-square (RMSECV) and four parameters of number of principal components (Factor) to investigate model performance, adopt prediction relative deviation (RSEP) to carry out the evaluation model predictive ability to unknown sample simultaneously, when R value is close to 1, when RPD value more than 2.5 and more big evaluation model performance more good, prediction accuracy is high, when RSEP value is less than 10%, evaluation model has good predictive ability, it is possible to meet the requirement that LIUWEI DIHUANG WAN concentrated pill crude drug powder quickly detects.
The modeling result that table 1 is the near-infrared model of 3 Testing index compares, as it can be seen from table 1 the near-infrared model of 3 Testing index is linear good, correlation coefficient is all more than 0.90, RPD value, more than 2.5, illustrates that the near-infrared quantitative calibration models effect set up is better.Relevant figure between measured value and the predictive value of moisture is shown in accompanying drawing 2, and the relevant figure between measured value and the predictive value of extract content is shown in accompanying drawing 3, and the relevant figure between measured value and the predictive value of Determination of Loganin is shown in accompanying drawing 4.
The each crucial Testing index content model parameter of table 1 LIUWEI DIHUANG WAN concentrated pill crude drug powder collects
| Model | R | RPD | RMSECV | Factors |
| Moisture model | 0.9871 | 6.24 | 0.104 | 6 |
| Extract content model | 0.9508 | 3.23 | 0.450 | 9 |
| Determination of Loganin model | 0.9208 | 2.56 | 0.005 | 9 |
(6) checking of calibration model
3 quantitative calibration models are respectively used to prediction checking and collect the content of moisture, extractum, loganin in sample.The measured value of moisture and near-infrared predictive value relatively see accompanying drawing 5, the measured value of extract content and near-infrared predictive value relatively see accompanying drawing 6, the content measured value of loganin and near-infrared predictive value compare sees accompanying drawing 7, it can be seen that the content measured value of 3 Testing index of LIUWEI DIHUANG WAN concentrated pill crude drug powder is close with near-infrared predictive value.
Table 2 is that the parameter that the near-infrared model of 3 different Testing index predicts the outcome collects, as can be seen from Table 2 moisture, loganin model RMSEP all below 1.0, moisture, extractum, Determination of Loganin model RSEP all within 10%, illustrate that the near-infrared analysis model of set up 3 Testing index has good predictive ability and stability.
The model prediction result of the table 2 LIUWEI DIHUANG WAN concentrated pill each Testing index of crude drug powder
| Model | RMSEP | RSEP (%) |
| Moisture model | 0.302 | 4.64 |
| Extract content model | 2.22 | 7.69 |
| Determination of Loganin model | 0.0191 | 7.66 |
(7) the near infrared light spectrum of LIUWEI DIHUANG WAN concentrated pill crude drug powder sample (140108,140109,140110 batches) to be measured is measured, steps for importing (5) positive model for school building, calculates the prediction content obtaining moisture in testing sample, extractum, loganin through model.
(8) above method is used to predict LIUWEI DIHUANG WAN concentrated pill crude drug powder moisture≤16.0% obtained, extract content >=24.0%, Determination of Loganin >=0.24%, then judge that this LIUWEI DIHUANG WAN concentrated pill crude drug powder is qualified samples, conform to quality requirements, it is possible to put into the subsequent production links such as extraction.
Assay method by the present embodiment step (2), measure batch 140108 (sample number into spectrum 1-5), 140109 (sample number into spectrum 6-10), the moisture of sample of 140110 (sample number into spectrum 11-15), extract content, Determination of Loganin value and near-infrared absorption spectrum value thereof respectively, near infrared spectrum value is imported the calibration model that the present embodiment step (5) is set up, the contrast table such as table 3 below of the prediction content obtaining moisture in testing sample, extractum, loganin, its predictive value and measured value is calculated through model:
The crucial Testing index measured value of table 3 LIUWEI DIHUANG WAN concentrated pill crude drug powder and predictive value
A kind of LIUWEI DIHUANG WAN concentrated pill crude drug powder multi objective express delivery detection method that the present invention proposes, it is shown that use this method can the moisture of LIUWEI DIHUANG WAN concentrated pill crude drug powder, extractum, Determination of Loganin quickly be analyzed.This method saves time, lossless, improve production efficiency and economic benefit, provide new method for the quality control of medical material, control its quality level from the beginning of production of LIUWEI DIHUANG WAN concentrated pill, it is ensured that finished dosage form safe and reliable.
Claims (10)
1. a LIUWEI DIHUANG WAN concentrated pill crude drug powder method for quick, it is characterised in that comprise the steps:
(1) the LIUWEI DIHUANG WAN concentrated pill crude drug powder of different production batch is gathered
(2) the crucial Testing index of LIUWEI DIHUANG WAN concentrated pill crude drug powder is measured
Choose moisture, extract content, Determination of Loganin as the crucial Testing index of LIUWEI DIHUANG WAN concentrated pill crude drug powder；
(3) LIUWEI DIHUANG WAN concentrated pill crude drug powder calibration set sample and the near-infrared original spectral data of checking collection sample are gathered
(4) pretreatment of near-infrared original spectrum
The calibration set sample near-infrared original spectrum that step (3) is gathered carries out pretreatment, with filter information, reduces noise；
(5) select the crucial Testing index modeling wave band of LIUWEI DIHUANG WAN concentrated pill crude drug powder, set up near infrared correction
(6) checking of calibration model
With the checking collection sample described in step (3), the calibration model described in step (5) is verified, after adopting the preprocess method identical with step (4) described calibration set sample near-infrared original spectrum, steps for importing (5) described calibration model, the performance of checking calibration model；
(7) measure the near infrared spectrum data of LIUWEI DIHUANG WAN concentrated pill crude drug powder sample to be measured, steps for importing (5) described calibration model, calculate the prediction content obtaining moisture in testing sample, extractum, loganin through model.
2. a kind of LIUWEI DIHUANG WAN concentrated pill crude drug powder method for quick according to claim 1, it is characterized in that described step (1) is gather the LIUWEI DIHUANG WAN concentrated pill crude drug powder sample of different production batch, medical material is after crushed, cross 80～120 mesh sieves, obtain even-grained LIUWEI DIHUANG WAN concentrated pill crude drug powder powder.
3. a kind of LIUWEI DIHUANG WAN concentrated pill crude drug powder method for quick according to claim 1, it is characterized in that described step (2) adopts moisture analysis content, cold-maceration is adopted to measure extract content, LIUWEI DIHUANG WAN concentrated pill crude drug powder, after pretreatment, adopts high effective liquid chromatography for measuring Determination of Loganin.
4. a kind of LIUWEI DIHUANG WAN concentrated pill crude drug powder method for quick according to claim 1, it is characterised in that described step (3) gathers the near-infrared original spectral data method of LIUWEI DIHUANG WAN concentrated pill crude drug powder calibration set sample and checking collection sample and is:
Precision weighs LIUWEI DIHUANG WAN concentrated pill crude drug powder medicinal powder 1～5g, is placed in culture dish, keeps powder surface smooth, adopts diffuse-reflectance method to gather near infrared spectrum, and with air for reference, scanning times is 1-640 time, and resolution is 2-16cm-1, scanning optical spectrum ranges for 4000-12000cm-1。
5. a kind of LIUWEI DIHUANG WAN concentrated pill crude drug powder method for quick according to claim 1, it is characterised in that the method for the pretreatment of described step (4) near-infrared original spectrum is:
The near-infrared original spectrum that step (3) is gathered carries out pretreatment, with filter information, reduces noise, including:
1) LIUWEI DIHUANG WAN concentrated pill crude drug powder moisture model adopts and deducts straight line pretreatment；
2) LIUWEI DIHUANG WAN concentrated pill crude drug powder extract content model adopts and eliminates constant offset Pretreated spectra；
3) the Determination of Loganin model of LIUWEI DIHUANG WAN concentrated pill crude drug powder adopts vector quantization normalizing (SNV) Pretreated spectra.
6. a kind of LIUWEI DIHUANG WAN concentrated pill crude drug powder method for quick according to claim 1, it is characterized in that selecting in described step (5) the crucial Testing index modeling wave band of LIUWEI DIHUANG WAN concentrated pill crude drug powder, the method setting up near-infrared quantitative model is:
By the near infrared spectrum of LIUWEI DIHUANG WAN concentrated pill crude drug powder calibration set sample after Pretreated spectra, its modeling waveband selection is as follows: water model modeling wave band is 9403.7-7498.3cm-1And 6102-4246.7cm-1；Extractum model modeling wave band is 7502.1-4597.7cm-1；Determination of Loganin model modeling wave band is 7502.1-4246.7cm-1, adopt partial least square method (PLS) to set up the quantitative calibration models between near infrared spectrum and above-mentioned each Testing index.
7. a kind of LIUWEI DIHUANG WAN concentrated pill crude drug powder method for quick according to claim 3, it is characterised in that described high effective liquid chromatography for measuring Determination of Loganin method is:
1) preprocess method is: take LIUWEI DIHUANG WAN concentrated pill crude drug powder (crossing 80-120 mesh sieve) about 0.5-1g, accurately weighed, puts in tool plug conical flask, precision adds 80% methanol of 30-100mL, it is heated to reflux 0.5-2h, is re-weighed, supply weightlessness with 80% methanol；Extracting solution is centrifuged 10min, and rotating speed is 10000-15000r min-1, take supernatant, both；
2) liquid phase chromatogram condition: chromatographic column: WatersCORTECSC18 analytical column (4.6 × 150mm, 2.7 μm)；Mobile phase is acetonitrile (B): water (A), gradient elution 0～10min:10～17%B, 10～15min:17～90%B；Detection wavelength 220-260nm, flow velocity is 0.8-1mL min-1, sample size is 5-25 μ L, column temperature 25-35 DEG C.
8. a kind of LIUWEI DIHUANG WAN concentrated pill crude drug powder method for quick according to claim 7, it is characterised in that described high effective liquid chromatography for measuring Determination of Loganin method is:
1) preprocess method is: take LIUWEI DIHUANG WAN concentrated pill crude drug powder (crossing 100 mesh sieves) about 0.5g, accurately weighed, puts in tool plug conical flask, and precision adds 80% methanol of 50mL, is heated to reflux 1h, is re-weighed, and supplies weightlessness with 80% methanol；Extracting solution is centrifugal 10min to the centrifuge tube of 1.5mL, and rotating speed is 13000r min-1, take supernatant, both；
2) liquid phase chromatogram condition: chromatographic column: WatersCORTECSC18 analytical column (4.6 × 150mm, 2.7 μm)；Mobile phase is acetonitrile (B): water (A), gradient elution 0～10min:10～17%B, 10～15min:17～90%B；Detection wavelength 240nm, flow velocity is 0.8mL min-1, sample size is 10 μ L, column temperature 30 DEG C.
9. a kind of LIUWEI DIHUANG WAN concentrated pill crude drug powder method for quick according to claim 4, it is characterised in that described scanning times is 32 times, and resolution is 8cm-1。
10. a kind of LIUWEI DIHUANG WAN concentrated pill crude drug powder multiple index quick detecting method according to claim 1, it is characterised in that:
The LIUWEI DIHUANG WAN concentrated pill crude drug powder multiple index quick detecting method described in claim 1 is used to measure the prediction content of the crucial Testing index in LIUWEI DIHUANG WAN concentrated pill crude drug powder, moisture≤16.0%, extract content >=24.0%, Determination of Loganin >=0.24% in the prediction content of the crucial Testing index of the LIUWEI DIHUANG WAN concentrated pill crude drug powder to be measured recorded, then judge that this LIUWEI DIHUANG WAN concentrated pill crude drug powder is qualified samples, conform to quality requirements, it is possible to put into the subsequent production links such as extraction.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109342358A (en) * | 2018-10-24 | 2019-02-15 | 吉林省现代中药工程研究中心有限公司 | The construction method and detection method of LIUWEIDIHUANG JIAONANG near-infrared quantitative calibration models |
| CN110609010A (en) * | 2019-09-06 | 2019-12-24 | 华润三九医药股份有限公司 | Method for rapidly determining content of components for radix zanthoxyli traditional Chinese medicine |
| CN111024643A (en) * | 2019-11-26 | 2020-04-17 | 中国科学院西北高原生物研究所 | Near infrared spectrum detection method for quality evaluation of gentiana straminea maxim medicinal materials |
| CN111650306A (en) * | 2020-07-07 | 2020-09-11 | 重庆医药高等专科学校 | HPLC method for simultaneously determining eight effective components in pill of six ingredients with rehmannia |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101101260A (en) * | 2007-05-25 | 2008-01-09 | 吉林大学 | Near infrared spectrum damage-free analysis method for anti-tuberculosis drugs |
| CN101303294A (en) * | 2008-06-20 | 2008-11-12 | 河南中医学院 | Application method of near-infrared on-line test technology in Chinese medicine Yiqing granule production |
| CN101485805A (en) * | 2009-02-27 | 2009-07-22 | 中南民族大学 | Quality control method of near-infrared holographic fingerprint for pills of six ingredients with rehmannia |
| CN101504362A (en) * | 2009-03-18 | 2009-08-12 | 哈尔滨商业大学 | Fast detection of trans-fatty acid content in edible fat based on near infrared spectrum technology |
| CN101664495A (en) * | 2009-09-17 | 2010-03-10 | 华东理工大学 | On-line detection method of near infrared spectrum for production process of traditional Chinese medicine, pill of six ingredients with rehmannia |
-
2014
- 2014-12-24 CN CN201410815047.3A patent/CN105784951B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101101260A (en) * | 2007-05-25 | 2008-01-09 | 吉林大学 | Near infrared spectrum damage-free analysis method for anti-tuberculosis drugs |
| CN101303294A (en) * | 2008-06-20 | 2008-11-12 | 河南中医学院 | Application method of near-infrared on-line test technology in Chinese medicine Yiqing granule production |
| CN101485805A (en) * | 2009-02-27 | 2009-07-22 | 中南民族大学 | Quality control method of near-infrared holographic fingerprint for pills of six ingredients with rehmannia |
| CN101504362A (en) * | 2009-03-18 | 2009-08-12 | 哈尔滨商业大学 | Fast detection of trans-fatty acid content in edible fat based on near infrared spectrum technology |
| CN101664495A (en) * | 2009-09-17 | 2010-03-10 | 华东理工大学 | On-line detection method of near infrared spectrum for production process of traditional Chinese medicine, pill of six ingredients with rehmannia |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109342358A (en) * | 2018-10-24 | 2019-02-15 | 吉林省现代中药工程研究中心有限公司 | The construction method and detection method of LIUWEIDIHUANG JIAONANG near-infrared quantitative calibration models |
| CN110609010A (en) * | 2019-09-06 | 2019-12-24 | 华润三九医药股份有限公司 | Method for rapidly determining content of components for radix zanthoxyli traditional Chinese medicine |
| CN111024643A (en) * | 2019-11-26 | 2020-04-17 | 中国科学院西北高原生物研究所 | Near infrared spectrum detection method for quality evaluation of gentiana straminea maxim medicinal materials |
| CN111024643B (en) * | 2019-11-26 | 2021-10-19 | 中国科学院西北高原生物研究所 | Near infrared spectrum detection method for quality evaluation of gentiana straminea maxim medicinal materials |
| CN111650306A (en) * | 2020-07-07 | 2020-09-11 | 重庆医药高等专科学校 | HPLC method for simultaneously determining eight effective components in pill of six ingredients with rehmannia |
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