CN101122586A - Pyrolysis gas chromatography analysis method for drug - Google Patents
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Abstract
The invention provides a cracking gas chromatography method used for drug identification. The steps of the method include that firstly, a drug is dissolved in organic solvent of water. Secondly, the cracking gas chromatography method is used to the drug detection. And a cracking gas chromatography fingerprint of the drug is obtained. Thirdly, the cracking gas chromatography fingerprints of the sample to be detected and a standard are respectively obtained through the first and the second step. And the sample is identified through the similarity analysis. The drug detection can be provided with a fast approach through the construction of a drug cracking gas chromatography database. The analyzing method provided by the invention is simple and accurate and provides an effective approach for the drug rapid detection and identification.
Description
Technical field
The present invention relates to a kind of analytical approach of medicine, particularly is a kind of method that pyrolysis gas chromatograph is differentiated medicine of using.
Background technology
At present, counterfeit and shoddy goods are very general on market in the medicine, and the situation complexity has and passes a fake product off as a genuine one, shoddy or the like.The good and bad true and false of medicine is directly connected to people's life security, so the quality assessment of medicine is extremely important.And drug inspection is mainly tested to finished product according to statutory standards.Have legal identity for some, be familiar with the professional fake producer of production technology and inspection technology again, be easy to bore the gap of test stone.As in Cortex Phellodendri capsule, adding quadracycline in " plum blossom K " case, illegally add " Chinese holly edge acid silaenafil " in the part medea, false orfloxacin capsule case that took place during fighting flood and relieve victims in 1998 or the like, all be that some legitimate enterprise are mixed other composition in official formula, to reduce cost, seek exorbitant profit.
Now, the basic skills of identification counterfeit drug mainly is to use multiple analysis means and method, comprehensive various assays, by with the comparison of known control sample parameter, counterfeit drug is discerned.Therefore, need the chronic of consumption, and need the amount of sample more relatively.When sample source difficulty, amount are little, and when requiring to differentiate fast, this discrimination method just a lot of problems occurred.Therefore, set up a kind of general, easy, differentiate that method for qualitative analysis is significant for the real and fake discrimination of medicine fast.
The pyrolytic gas chromatography method is simple because of sample pre-treatments, consumption is few, easyly come into one's own fast, has been widely used in the evaluation of protein, microorganism in pharmaceutical field, has been proved to be a kind of efficient ways.Compared with other routine inspection analytical approach such as HPLC, GC, TLC etc., pyrolysis gas chromatography has and is applicable to various sample analysis, advantage such as pre-service is simple, and cost is low, and amount of samples is few, highly sensitive, and analysis speed is fast.But also neither one can for reference and efficient ways at the detection range of medicine.
Summary of the invention
(1) technical matters that will solve
The objective of the invention is to disclose a kind of pyrolytic gas chromatography method of medicine, be used for differentiating rapidly and accurately different medicines.
(2) technical scheme
For achieving the above object, concrete technical scheme of the present invention is:
1. medicine is dissolved in the organic solvent of water;
2. use pyrolysis gas chromatography medicine is measured, obtain the pyrolysis gas chromatograph figure of medicine;
3. obtain the pyrolysis gas chromatograph collection of illustrative plates of testing sample and standard items by step 1,2 respectively, and differentiate sample by similarity analysis.
And can pass through step 1 and 2, set up standard medicine pyrolysis gas chromatograph database (hereinafter to be referred as database), the pyrolysis gas chromatograph collection of illustrative plates of medicine to be measured and the collection of illustrative plates in the database be compared analysis can differentiate medicine.
In step (1), the organic solvent of described water, wherein the content of water is 0～5: 10 by volume; Described organic solvent is for often being applied to the solvent of medicine dissolving, and be preferably and be selected from following group: acetonitrile, chlorobenzene, chloroform, methylene chloride, normal hexane, methyl alcohol, formamide, phenixin, pyridine, toluene, butanone, ether, acetate, acetone, methyl cyclic group alkane, methoxybenzene, normal butyl alcohol, cumene, ethanol, ethyl acetate, formic acid, isooctane, N, N-dimethoxy acetamide, N, N-dimethoxy formamide, with and composition thereof; Not diffluent medicine can be used the ultrasound wave hydrotropy.
In step (2), the crack temperature range of medicine is 300 ℃～1000 ℃ in the pyrolysis gas chromatography, and the cracking pressure limit is 10.0psi～50.0psi; Chromatographic column in the analytical conditions for gas chromatography is preferably and is selected from following group: SPB-1, DB-624 or HP-FFAP, wherein the heating rate scope of chromatographic column is 3～20 ℃/min.
Above-mentioned database can comprise two parts, one is two powers peak data storehouses, it is as reference with the strongest chromatographic peak in the sample, calculate the relative retention value of two the strongest in sample components, and the retention time of two components is arranged in order the database of setting up successively by ascending order; Another is to compose database entirely, it is as external standard with tetralin, calculate the relative retention value and the relative peak area ratio of each component in the sample, and the relative retention value α of each component in the sample is arranged in order by ascending order, set up cracking gas phase fingerprints database with this.
Comprise penicillins and cephalo-type in the database of having set up at present: penicillins: Cloxacillin Lenampicillin Oxacillin Sultamicillin flucloxacillin, ospeneff mezlocillin, Amoxicillin, benzylpenicillin potassium ampicillin Piperacillin cephalo-type: cefalexin cefadroxil Cefradine cefotaxime Cefaclor cefoxitin cefoperazone CTX CEFUROXIME AXETIL cephazoline cefathiamidine
Used similarity analysis software is chromatographic fingerprints of Chinese materia medica similarity evaluation system (2004A version, Chinese Pharmacopoeia Commission) among the present invention, and it calculates principle is included angle cosine.
(3) beneficial effect
The invention discloses the pyrolysis gas chromatography analysis method of medicine, the consumption of its sample is few, can directly use the sample of any physical aspect to measure, avoided losing of the analysis distortion that may bring or other information because of pre-service, simple to operate, highly sensitive, for the fast detecting of medicine, differentiate efficient ways is provided.
Description of drawings
Fig. 1 is a different manufacturers Benzylpenicillin sodium salt finger-print;
Fig. 2 is a different manufacturers cefalexin finger-print;
Fig. 3 is a different manufacturers Cefradine finger-print;
Fig. 4 is a different manufacturers ampicillin sodium finger-print;
Fig. 5 is a different manufacturers Amoxicillin Sodium finger-print;
Fig. 6 is the finger-print of sample 041001;
Fig. 7 is the finger-print of sample 041002;
Fig. 8 is the finger-print of sample 041003.
Embodiment
The present invention is further illustrated below in conjunction with embodiment, but be not used for limiting invention which is intended to be protected.
Used microbiotic reference substance (standard items) is Nat'l Pharmaceutical ﹠ Biological Products Control Institute among the embodiment provides.
Benzylpenicillin sodium for injection, standard items
Huabei Pharmaceutic Co., Ltd
Shijiazhuang Pharmaceutical Group Co Ltd
Shangdong Ruiyang Pharmaceutical Co., Ltd
Solvent: the methanol solution of water, wherein the volume ratio of water and methyl alcohol is 2: 8
Medicine is dissolved in the above-mentioned solvent, and the solution that is mixed with 1mg/ml is as need testing solution.
The pyrolysis gas chromatograph experiment condition is as follows:
Carrier gas: nitrogen, flow velocity 2.0ml/min; Detecting device is flame ionization ditector (FID); Hydrogen flow rate 30ml/min; Air velocity 300ml/min; Split ratio 1: 1, sample size: 2 μ l.
Chromatographic column: HP-FFAP, 30m * 0.32mm, 0.25 μ m, immobile liquid are that polyglycol-nitro terephthalic acid (TPA) is modified;
Temperature programme: initial temperature: 60 ℃; Retention time: 8min
Heating rate: 10 ℃/min
Terminal temperature: 240 ℃; Retention time: 20min
Injector temperature: 240 ℃; Detector temperature: 260 ℃
Cracker temperature: 300 ℃
Cracking pressure: 14.0psi
Its pyrolysis gas chromatograph finger-print as shown in Figure 1, similarity result is as shown in table 1.
Wherein, S1 is a standard diagram; S2. Shandong; S3. Shijiazhuang; S4. North China.
Table 1 benzylpenicillin sodium for injection similarity result
| S1 | S2 | S3 | S4 | |
| S1 | 1.000 | |||
| S2 | 0.975 | 1.000 | ||
| S3 | 0.963 | 0.918 | 1.000 | |
| S4 | 0.982 | 0.975 | 0.963 | 1.000 |
Between the two the similarity of each numeric representation for intersecting in the table 1, as 0.975 similarity that just is expressed as between S1 and the S2, and wherein same collection of illustrative plates of 1.000 expressions compares.The collection of illustrative plates of three producers and the similarity between the standard diagram are fine as can be seen from the table, and the similarity value thinks that all more than 0.95 their materials corresponding with standard diagram are same substance, promptly all is penicillin.
Cefalexin, standard items
Beijing Hua Feng drugmaker
The Qingjian River, Jiangxi pharmaceutical factory
Tangshan the emperor's kindness pharmaceutcal corporation, Ltd
Solvent: the methanol solution of water, wherein the volume ratio of water and methyl alcohol is 1: 2
With above-mentioned tablet porphyrize, take by weighing in right amount, use above-mentioned dissolution with solvents, use 0.45 μ m membrane filtration again, get subsequent filtrate.
The pyrolysis gas chromatograph experiment condition is as follows:
Carrier gas: nitrogen, flow velocity 2.0ml/min; Detecting device is flame ionization ditector (FID); Hydrogen flow rate 30ml/min; Air velocity 300ml/min; Split ratio 1: 1, sample size: 2 μ l.
Chromatographic column: SPB-1,30m * 0.32mm, 0.25 μ m, immobile liquid are that polyglycol-nitro terephthalic acid (TPA) is modified;
Temperature programme: initial temperature: 60 ℃; Retention time: 8min
Heating rate: 3 ℃/min
Terminal temperature: 240 ℃; Retention time: 20min
Injector temperature: 240 ℃; Detector temperature: 260 ℃
Cracker temperature: 300 ℃
Cracking pressure: 10.0psi
Its pyrolysis gas chromatograph finger-print as shown in Figure 2, similarity result is as shown in table 2.
Wherein, S5 is a standard diagram; S6. Jiangxi; S7. Tangshan; S8. Beijing.
Table 2 cefalexin Tablet similarity result
| S5 | S6 | S7 | S8 | |
| S5 | 1.000 | |||
| S6 | 0.915 | 1.000 | ||
| S7 | 0.827 | 0.861 | 1.000 | |
| S8 | 0.830 | 0.849 | 0.850 | 1.000 |
As seen from Table 2, sample and standard diagram similarity value are all more than 0.8, and similarity is better.Wherein, with the reference substance similarity the highest be S6.
Cefradine, standard items
HARBIN PHARMACEUTICAL GROUP CO., LTD. General Pharm. Factory
Fujian Gutian Pharmaceutical Co., Ltd.
The former branch office in Lukang Medical Co., Ltd., Shandong Shandong
Solvent: the methanol solution of water, wherein the volume ratio of water and methyl alcohol is 1: 5
Cefradine, standard items
HARBIN PHARMACEUTICAL GROUP CO., LTD. General Pharm. Factory
Fujian Gutian Pharmaceutical Co., Ltd.
The former branch office in Lukang Medical Co., Ltd., Shandong Shandong
It is an amount of to take by weighing capsule 's content, uses above-mentioned dissolution with solvents, uses 0.45 μ m membrane filtration again, gets subsequent filtrate.
The pyrolysis gas chromatograph experiment condition is as follows:
Carrier gas: nitrogen, flow velocity 2.0ml/min; Detecting device is flame ionization ditector (FID); Hydrogen flow rate 30ml/min; Air velocity 300ml/min; Split ratio 1: 1, sample size: 2 μ l.
Chromatographic column: HP-FFAP, 30m * 0.32mm, 0.25 μ m, immobile liquid are that polyglycol-nitro terephthalic acid (TPA) is modified;
Temperature programme: initial temperature: 60 ℃; Retention time: 8min
Heating rate: 20 ℃/min
Terminal temperature: 240 ℃; Retention time: 20min
Injector temperature: 240 ℃; Detector temperature: 260 ℃
Cracker temperature: 1000 ℃
Cracking pressure: 50.0psi
Its pyrolysis gas chromatograph finger-print as shown in Figure 3, similarity result is as shown in table 3.
Wherein, S9 is a standard diagram; S10. Fujian; S11. breathe out medicine; S12. Shandong.
Table 3 Cefradine capsule similarity result
| S9 | S10 | S11 | S12 | |
| S9 | 1.000 | |||
| S10 | 0.930 | 1.000 | ||
| S11 | 0.941 | 0.952 | 1.000 | |
| S12 | 0.946 | 0.949 | 0.938 | 1.000 |
As seen from Table 3, the collection of illustrative plates similarity value of sample and standard is all more than 0.9, and similarity is better.Wherein, with the reference substance similarity the highest be S12.
Test example 4: powder ampoule agent for injection ampicillin sodium
Ampicillin sodium, standard items
Huabei Pharmaceutic Co., Ltd
A day biological pharmaceutcal corporation, Ltd converges in Fujian
Solvent: the methanol solution of water, wherein the volume ratio of water and methyl alcohol is 1: 3
Medicine is dissolved in the above-mentioned solvent, and the solution that is mixed with 1mg/ml is as need testing solution.
The pyrolysis gas chromatograph experiment condition is as follows:
Carrier gas: nitrogen, flow velocity 2.0ml/min; Detecting device is flame ionization ditector (FID); Hydrogen flow rate 30ml/min; Air velocity 300ml/min; Split ratio 1: 1, sample size: 2 μ l.
Chromatographic column: HP-FFAP, 30m * 0.32mm, 0.25 μ m, immobile liquid are that polyglycol-nitro terephthalic acid (TPA) is modified;
Temperature programme: initial temperature: 60 ℃; Retention time: 8min
Heating rate: 15 ℃/min
Terminal temperature: 240 ℃; Retention time: 20min
Injector temperature: 240 ℃; Detector temperature: 260 ℃
Cracker temperature: 500 ℃
Cracking pressure: 20.0psi
Its pyrolysis gas chromatograph finger-print as shown in Figure 4, similarity result is as shown in table 4.Wherein, S13. is a standard diagram; S14. North China; S15. converge day in Fujian.
Table 4 ampicillin for inj sodium similarity result table
| S13 | S14 | S15 | |
| S13 | 1.000 | 0.917 | 0.874 |
| S14 | 0.917 | 1.000 | 0.952 |
| S15 | 0.874 | 0.952 | 1.000 |
As shown in Table 4, S14 and standard items are more approaching.
Test example 5: powder ampoule agent for injection Amoxicillin Sodium
Amoxicillin Sodium, standard items
Hainan Province Hai Ling pharmaceutical factory
HARBIN PHARMACEUTICAL GROUP CO., LTD. General Pharm. Factory
Solvent: the methanol solution of water, wherein the volume ratio of water and methyl alcohol is 1: 9
Medicine is dissolved in the above-mentioned solvent, and the solution that is mixed with 1mg/ml is as need testing solution.
The pyrolysis gas chromatograph experiment condition is as follows:
Carrier gas: nitrogen, flow velocity 2.0ml/min; Detecting device is flame ionization ditector (FID); Hydrogen flow rate 30ml/min; Air velocity 300ml/min; Split ratio 1: 1, sample size: 2 μ l.
Chromatographic column: HP-FFAP, 30m * 0.32mm, 0.25 μ m, immobile liquid are that polyglycol-nitro terephthalic acid (TPA) is modified;
Temperature programme: initial temperature: 60 ℃; Retention time: 8min
Heating rate: 18 ℃/min
Terminal temperature: 240 ℃; Retention time: 20min
Injector temperature: 240 ℃; Detector temperature: 260 ℃
Cracker temperature: 650 ℃
Cracking pressure: 30.0psi
Its pyrolysis gas chromatograph finger-print as shown in Figure 5, similarity result is as shown in table 5.Wherein, S16 is standard items, and S17 is Hainan, and S18 is for breathing out medicine.
Table 5 Amoxicillin Sodium similarity result table
| S16 | S17 | S18 | |
| S16 | 1.000 | 0.914 | 0.930 |
| S17 | 0.914 | 1.000 | 0.955 |
| S18 | 0.930 | 0.955 | 1.000 |
It can be seen from the table, the collection of illustrative plates similarity value of sample and standard is all more than 0.9, and the similarity between sample and the standard is better.
The foundation of embodiment 6 databases
The foundation of penicillins cracking gas phase fingerprints database is example with benzylpenicillin potassium, ampicillin and Amoxicillin:
Because the pyrolysis gas chromatograph finger-print is complicated, directly the comparing data amount is big, retrieve more complicated, therefore, wish to make up one by preliminary screening to final definite retrieval flow, promptly at first carry out scalping, dwindle range of search by two the strongest in the spectrogram peak-to-peak relative retention values of chromatogram; And then compose comparison entirely, final definite.
Solvent: the hexane solution of water, wherein the volume ratio of water and normal hexane is 1: 3
Medicine is dissolved in the above-mentioned solvent, and the solution that is mixed with 1mg/ml is as need testing solution.
The pyrolysis gas chromatograph experiment condition is as follows:
Carrier gas: nitrogen, flow velocity 2.0ml/min; Detecting device is flame ionization ditector (FID); Hydrogen flow rate 30ml/min; Air velocity 300ml/min; Split ratio 1: 1, sample size: 2 μ l.
Chromatographic column: HP-FFAP, 30m * 0.32mm, 0.25 μ m, immobile liquid are that polyglycol-nitro terephthalic acid (TPA) is modified;
Temperature programme: initial temperature: 60 ℃; Retention time: 8min
Heating rate: 15 ℃/min
Terminal temperature: 240 ℃; Retention time: 20min
Injector temperature: 240 ℃; Detector temperature: 260 ℃
Cracker temperature: 500 ℃
Cracking pressure: 20.0psi
Two powers peak data storehouse:
With the strongest chromatographic peak in the sample is reference, calculates the relative retention value of two the strongest in sample components, and the retention time of two components is arranged in order by ascending order, sets up two powers peak data storehouse with this, sees Table 6.
Table 6 penicillins two powers peak data storehouse
| Component | T＝400℃ | T＝600℃ | T＝800℃ | |||
| T | α | T | α | T | α | |
| Benzylpenicillin potassium | 25.78 | 0.934 | 17.13 | 0.615 | - | - |
| 27.60 | 1.000 | 27.85 | 1.000 | |||
| The ampicillin | 14.88 | 0.846 | 13.52 | 1.000 | 5.67 | 0.382 |
| 17.59 | 1.000 | 14.89 | 1.101 | 14.82 | 1.000 | |
| The Amoxicillin | 17.59 | 1.000 | 20.46 | 1.000 | 20.31 | 1.000 |
| 20.35 | 1.157 | 21.33 | 1.042 | 21.27 | 1.047 | |
Full spectrum database:
As external standard, calculate the relative retention value and the relative peak area ratio of each component in the sample with tetralin, and the relative retention value α of each component in the sample is arranged in order by ascending order, set up cracking gas phase fingerprints database, see Table 7 with this.
Table 7 penicillins database
| Component | T＝400℃ | T＝600℃ | T＝800℃ | ||||||
| T | α | Ar | T | α | Ar | T | α | Ar | |
| Tetralin | 12.92 | 1.000 | 1.00 | 12.74 | 1.000 | 1.00 | 16.94 | 1.000 | 1.00 |
| Benzylpenicillin potassium | 17.06 17.62 17.81 17.97 19.80 20.47 25.78 27.16 27.60 | 1.321 1.364 1.379 1.391 1.533 1.585 1.996 2.103 2.137 | 0.456 0.249 0.085 0.516 0.137 0.033 0.331 0.205 3.312 | 5.01 5.61 17.13 17.92 19.41 19.85 27.57 27.85 | 0.393 0.440 1.345 1.407 1.523 1.558 2.164 2.186 | 0.658 0.184 0.267 0.237 0.157 0.401 0.158 0.425 | - | - | - |
| The ampicillin | 13.62 14.88 17.59 17.79 17.93 25.90 27.50 27.75 28.12 30.80 | 1.055 1.152 1.362 1.377 1.388 2.005 2.129 2.148 2.177 2.384 | 0.155 0.327 0.484 0.169 0.367 0.053 0.068 0.159 0.064 0.074 | 4.98 13.45 13.52 14.89 17.14 19.41 | 0.391 1.055 1.061 1.168 1.345 1.523 | 1.015 0.136 1.570 1.365 0.061 0.077 | 5.67 12.49 13.64 14.82 15.69 17.08 19.43 | 0.335 0.737 0.805 0.875 0.926 1.009 1.147 | 2.567 1.042 1.813 23.73 1.314 0.561 0.668 |
| The Amoxicillin | 17.59 17.78 17.98 20.35 | 1.362 1.376 1.392 1.576 | 0.447 0.160 0.253 0.608 | 5.02 5.18 20.46 21.33 | 0.394 0.406 1.606 1.674 | 0.807 0.581 1.352 1.004 | 14.92 20.31 21.27 34.28 | 0.881 1.199 1.256 2.024 | 3.75 20.11 10.57 1.55 |
Annotate: "-" expression does not have feature pyrolysis gas chromatograph peak
Embodiment 7 application data bases are analyzed medicine
The sample that is denoted as ampicillin sodium is analyzed with database.
The powder ampoule agent for injection ampicillin sodium
Ampicillin sodium, 041001
041002
041003
Solvent: the hexane solution of water, wherein the volume ratio of water and normal hexane is 1: 3
Medicine is dissolved in the above-mentioned solvent, and the solution that is mixed with 1mg/ml is as need testing solution.
The pyrolysis gas chromatograph experiment condition is with embodiment 6.
Its pyrolysis gas chromatograph finger-print as shown in the figure,
As we know from the figure, do not have the pyrolysis chromatography peak in sample 041001 collection of illustrative plates, it is not an ampicillin sodium certainly;
Two powers' peak data table of listing sample 041002 and 041003 sees Table 1
Table 1
| Component | T＝400℃ | |
| T | α | |
| The ampicillin | 14.88 | 0.846 |
| 17.59 | 1.000 | |
| 041002 | 25.48 | 0.921 |
| 27.67 | 1.000 | |
| 041003 | 14.84 | 0.843 |
| 17.61 | 1.000 | |
As can be known from Table 1, sample 041003 is more close with ampicillin two powers peak data, and it is composed comparison entirely, calculates similarity, sees Table 2
Table 2
| The ampicillin | 041003 | |
| The ampicillin | 1.000 | |
| 041003 | 0.915 | 1.000 |
As seen from Table 2, sample 041003 is better with the standard diagram similarity of ampicillin, and tentatively judgement sample 041003 is the ampicillin.
Claims (5)
1. the pyrolytic gas chromatography method of a medicine is characterized in that comprising the steps:
(1) with sample dissolution in the organic solvent of water;
(2) use pyrolysis gas chromatography medicine is measured, obtain the pyrolysis gas chromatograph finger-print of medicine;
(3) obtain the pyrolysis gas chromatograph finger-print of sample and standard items respectively by step (1) and (2), and pass through both similarities of similarity software analysis.
2. the pyrolytic gas chromatography method of a medicine, it is characterized in that by set up the pyrolysis gas chromatograph fingerprints database of standard medicine by the step in the claim 1 (1) and (2), and applications similar degree analysis software is differentiated medicine with comparing in the pyrolysis gas chromatograph finger-print of sample and the database.
3. method according to claim 2, it is characterized in that described pyrolysis gas chromatograph fingerprints database comprises that with the strongest chromatographic peak in the standard medicine be reference, calculate the relative retention value of two the strongest in medicine components, and the retention time of two components is arranged in order by ascending order, with this two powers peak data storehouse of setting up; And, with tetralin as external standard, calculate the relative retention value and the relative peak area ratio of each component in the sample, and the relative retention value α of each component in the sample is arranged in order by ascending order, compose database entirely with this cracking gas-phase fingerprint pattern of setting up.
4. pyrolysis gas chromatography analysis method according to claim 1 and 2, it is characterized in that, the water of the organic solvent of described water is 0～5: 10 with the volume of organic solvent ratio, wherein, described organic solvent is acetonitrile, chlorobenzene, chloroform, methylene chloride, normal hexane, methyl alcohol, formamide, phenixin, pyridine, toluene, butanone, ether, acetate, acetone, methyl cyclic group alkane, methoxybenzene, normal butyl alcohol, cumene, ethanol, ethyl acetate, formic acid, isooctane, N, N-dimethoxy acetamide, N, any one or more in the N-dimethoxy formamide.
5. pyrolysis gas chromatography analysis method according to claim 1 and 2, it is characterized in that, the cracking temperature of medicine is 300 ℃～1000 ℃ in the pyrolysis gas chromatography, cracking pressure is 10.0psi～50.0psi, chromatographic column is any among SPB-1, DB-624 or the HP-FFAP, and the heating rate scope of chromatographic column is 3～20 ℃/min.
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| CN106596821A (en) * | 2016-12-12 | 2017-04-26 | 中国测试技术研究院 | Quick determination method of organic solvents in pesticide preparation |
| CN106596821B (en) * | 2016-12-12 | 2018-07-20 | 中国测试技术研究院 | The rapid assay methods of organic solvent in a kind of pesticidal preparations |
| CN109507355A (en) * | 2019-01-17 | 2019-03-22 | 浙江工业大学 | The method of methamphetamine and head-shaking pill content in Flash evaporation gas chromatography mass spectrometric determination human hair |
| CN110470776A (en) * | 2019-07-31 | 2019-11-19 | 广东药科大学 | The screening method of illegal additive in a kind of ginseng pills of sea dog |
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