CN106442841A - Separation and detection method of cationic surface active agent in medicine - Google Patents
Separation and detection method of cationic surface active agent in medicine Download PDFInfo
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- 239000003814 drug Substances 0.000 title claims abstract description 96
- 238000000926 separation method Methods 0.000 title claims abstract description 26
- 239000004094 surface-active agent Substances 0.000 title claims abstract description 18
- 238000001514 detection method Methods 0.000 title abstract description 13
- 125000002091 cationic group Chemical group 0.000 title abstract description 4
- 239000007789 gas Substances 0.000 claims abstract description 80
- 238000000034 method Methods 0.000 claims abstract description 66
- 239000012488 sample solution Substances 0.000 claims abstract description 58
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000012159 carrier gas Substances 0.000 claims abstract description 27
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 15
- 239000000523 sample Substances 0.000 claims abstract description 15
- 229940079593 drug Drugs 0.000 claims description 56
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 claims description 29
- 239000003093 cationic surfactant Substances 0.000 claims description 28
- 238000002360 preparation method Methods 0.000 claims description 26
- 239000003085 diluting agent Substances 0.000 claims description 24
- 230000004907 flux Effects 0.000 claims description 19
- 238000002347 injection Methods 0.000 claims description 19
- 239000007924 injection Substances 0.000 claims description 19
- 239000000203 mixture Substances 0.000 claims description 18
- 238000000855 fermentation Methods 0.000 claims description 17
- 230000004151 fermentation Effects 0.000 claims description 17
- -1 polysiloxanes Polymers 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 229920002385 Sodium hyaluronate Polymers 0.000 claims description 12
- 239000001257 hydrogen Substances 0.000 claims description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims description 12
- 229940010747 sodium hyaluronate Drugs 0.000 claims description 12
- YWIVKILSMZOHHF-QJZPQSOGSA-N sodium;(2s,3s,4s,5r,6r)-6-[(2s,3r,4r,5s,6r)-3-acetamido-2-[(2s,3s,4r,5r,6r)-6-[(2r,3r,4r,5s,6r)-3-acetamido-2,5-dihydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-2-carboxy-4,5-dihydroxyoxan-3-yl]oxy-5-hydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-3,4,5-trihydroxyoxane-2- Chemical compound [Na+].CC(=O)N[C@H]1[C@H](O)O[C@H](CO)[C@@H](O)[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@H](O[C@H]2[C@@H]([C@@H](O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@H](O3)C(O)=O)O)[C@H](O)[C@@H](CO)O2)NC(C)=O)[C@@H](C(O)=O)O1 YWIVKILSMZOHHF-QJZPQSOGSA-N 0.000 claims description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 11
- 238000007664 blowing Methods 0.000 claims description 11
- 229920001296 polysiloxane Polymers 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000000834 fixative Substances 0.000 claims description 9
- 238000013329 compounding Methods 0.000 claims description 7
- DDXLVDQZPFLQMZ-UHFFFAOYSA-M dodecyl(trimethyl)azanium;chloride Chemical group [Cl-].CCCCCCCCCCCC[N+](C)(C)C DDXLVDQZPFLQMZ-UHFFFAOYSA-M 0.000 claims description 7
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 7
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 6
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 6
- VBIIFPGSPJYLRR-UHFFFAOYSA-M Stearyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCC[N+](C)(C)C VBIIFPGSPJYLRR-UHFFFAOYSA-M 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 125000000217 alkyl group Chemical group 0.000 claims description 4
- 235000019270 ammonium chloride Nutrition 0.000 claims description 4
- 150000001768 cations Chemical class 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 150000001335 aliphatic alkanes Chemical group 0.000 claims description 2
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims description 2
- 238000010189 synthetic method Methods 0.000 claims description 2
- AJXBTRZGLDTSST-UHFFFAOYSA-N amino 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)ON AJXBTRZGLDTSST-UHFFFAOYSA-N 0.000 claims 1
- 238000012360 testing method Methods 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 15
- 239000000243 solution Substances 0.000 description 14
- 238000005516 engineering process Methods 0.000 description 13
- 238000004519 manufacturing process Methods 0.000 description 13
- 230000004044 response Effects 0.000 description 13
- 238000010812 external standard method Methods 0.000 description 12
- 239000013558 reference substance Substances 0.000 description 11
- 230000008569 process Effects 0.000 description 10
- 238000004458 analytical method Methods 0.000 description 7
- 239000007788 liquid Substances 0.000 description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 6
- 150000003863 ammonium salts Chemical class 0.000 description 6
- 239000012490 blank solution Substances 0.000 description 6
- 238000004128 high performance liquid chromatography Methods 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 125000005210 alkyl ammonium group Chemical group 0.000 description 3
- 238000005660 chlorination reaction Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 239000010414 supernatant solution Substances 0.000 description 3
- WWSNLNXXISONLQ-UHFFFAOYSA-N C(CCCCCCCCCCCCCCC)Cl(C)(C)C Chemical compound C(CCCCCCCCCCCCCCC)Cl(C)(C)C WWSNLNXXISONLQ-UHFFFAOYSA-N 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- DCAYPVUWAIABOU-UHFFFAOYSA-N hexadecane Chemical compound CCCCCCCCCCCCCCCC DCAYPVUWAIABOU-UHFFFAOYSA-N 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 125000004433 nitrogen atom Chemical group N* 0.000 description 2
- 150000007524 organic acids Chemical class 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- PXFBZOLANLWPMH-UHFFFAOYSA-N 16-Epiaffinine Natural products C1C(C2=CC=CC=C2N2)=C2C(=O)CC2C(=CC)CN(C)C1C2CO PXFBZOLANLWPMH-UHFFFAOYSA-N 0.000 description 1
- MPNXSZJPSVBLHP-UHFFFAOYSA-N 2-chloro-n-phenylpyridine-3-carboxamide Chemical compound ClC1=NC=CC=C1C(=O)NC1=CC=CC=C1 MPNXSZJPSVBLHP-UHFFFAOYSA-N 0.000 description 1
- UKSCCFZEWXIOKE-UHFFFAOYSA-N 5-azido-2,3-dibromo-6-phenyl-4-phenyldiazenylbenzoic acid Chemical compound BrC1=C(C(=C(C(=C1N=NC1=CC=CC=C1)N=[N+]=[N-])C1=CC=CC=C1)C(=O)O)Br UKSCCFZEWXIOKE-UHFFFAOYSA-N 0.000 description 1
- 241000208340 Araliaceae Species 0.000 description 1
- JBPBWEKERUNUQY-UHFFFAOYSA-N C(CCCCCCCCCCCCCCCCC)Cl(C)(C)C Chemical compound C(CCCCCCCCCCCCCCCCC)Cl(C)(C)C JBPBWEKERUNUQY-UHFFFAOYSA-N 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 125000005211 alkyl trimethyl ammonium group Chemical group 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 239000013068 control sample Substances 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 125000000623 heterocyclic group Chemical group 0.000 description 1
- 125000001165 hydrophobic group Chemical group 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 238000001819 mass spectrum Methods 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 210000000952 spleen Anatomy 0.000 description 1
- 210000002784 stomach Anatomy 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analysing Biological Materials (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention provides a separation and detection method of a cationic surface active agent in medicine.The method comprises the following steps of preparing a medicine sample solution; injecting the prepared medicine sample solution into a gas chromatograph, and separating and detecting in the following conditions; chromatographic conditions: nitrogen is used as carrier gas, and the carrier gas flow is controlled to be 2 mL/min to 8 mL/min; the temperature of a sample inlet of the gas chromatograph is 250 DEG C to 300 DEG C; the temperature of an FTD (Flame Thermionic Detector) is 250 DEG C to 320 DEG C; the column temperature of the gas chromatograph: the initial temperature of 90 DEG C to 150 DEG C is kept for 2 min to 5 min, and the temperature is increased to 240 DEG C to 260 DEG C at the speed of 10 DEG C/min to 15 DEG C/min and is kept for 4 min to 7 min. According to the method, the cationic surface active agent in a medicine sample is separated or detected by the gas chromatograph in the special chromatographic conditions, and the method has the advantages of high precision and good repeatability.
Description
Technical field
The invention belongs to analysis mensure field, it is related to a kind of method for separating and detecting, more particularly, to a kind of medicine cationic
The method for separating and detecting of surfactant.
Background technology
The surface-active ion generating when cationic surfactant ionizes in aqueous is positively charged, its hydrophobic group with
Anion surfactant is similar.Contain nitrogen-atoms in the hydrophilic group ion of cationic surfactant, divided according to nitrogen-atoms
Position difference in son is divided into amine salt, quaternary ammonium salt and heterocyclic type three class.
Quaternary cationicses good water solubility, not only acidproof but also alkaline-resisting and great majority have bactericidal action.Use season
Ammonium salt cationic surfactant can affine with many materials, absorption formed hydrogen bond, have turbidity removal, decolouring, absorption and bond etc.
, it is adaptable to purifying process in the industry such as fermentation pharmacy, application is widely for function.
Sodium Hyaluronate is a kind of crude drug, using hexadecyltrimethylammonium chloride (CTAC) this season in its technique productions
Ammonium salt cationoid surfactant is as chelating agent, in view of the safety in utilization of product considers, residual quantity should be tight in the product
Lattice control, and therefore how to realize to the separation of the surfactant such as ammonium salt cationic surfactant and detection in medicine is very
Important.
Because of it, there is the features such as not volatile, polarity is strong for most of ammonium salt cationoid surfactants, generally adopt
Carry out quantitative analyses with liquid chromatograph, for example with the high performance liquid chromatography connecting DAD detector (diode array detector)
Method carries out quantitative analyses, but as alkylammonium salt cationoid surfactant does not have chromophore, therefore can not often directly use
The high performance liquid chromatograph device of the connection DAD detector of rule or fluorescence detector is analyzed.
Research shows, can be to the alkyl not having chromophore using the HPLC (high performance liquid chromatography) connecting electric conductivity detector
Ammonium salt cationoid surfactant carries out detection by quantitative.As CN 102226796A discloses a kind of mensure amophoteric surface active
Micro N in agent, the analysis method of N- dimethylated propyl diethylenetriamine, the method is analyzed using the chromatography of ions, chromatographic test strip part
As follows：Chromatographic column：Cation chromatographic column；Mobile phase：The mineral acid being 70%～100% by volumn concentration or organic acid acid
Aqueous solution and organic solvent that volumn concentration is 0%～30% composition, described mineral acid or aqueous solutions of organic acids mole
Concentration is 1mmol/L～10mmol/L；Detector：Using electric conductivity detector；Flow rate of mobile phase：0.5mL/min～1.5mL/
min.
Additionally by adding organic reagent such as dibromo carboxyl phenyl diazoaminoazobenzene, with alkylammonium in alkaline medium
There is association chromogenic reaction in salt cationic surfactant, then be analyzed being also a kind of detection alkane by spectrophotography
The method of base ammonium salt cationoid surfactant.
However, said method have qualitative, quantitative effect when haveing the shortcomings that interfering material poor.
Connect high performance liquid chromatography using atmospheric pressure electrospray simpleness method (ESI/MS) to be analyzed, provided according to mass spectrum
Molecular weight information carries out qualitative to its structure and composition, carries out quantitative analyses using high performance liquid chromatography, can be accurately qualitative and fixed
Quantify two or more mixed surfactants, but detecting instrument used by this method is expensive, relatively costly.
And, it is more complicated due to forming in medicine, when Surfactant carries out separation determination due to other components
Interference, be difficult to accomplish that Surfactant is accurately separated and measures.
Therefore, how to seek one kind and can effectively measure medicine cationic surfactant, especially alkylammonium salt
Cationic surfactant, and the little method of cost is necessary.
Content of the invention
Poor for qualitative, quantitative effect present in existing cationic surfactant analysis determining method, and instrument price
Costliness, high cost, and the problems such as separate currently for materials such as surfactants in medicine and measure difficult, the present invention provides
A kind of method for separating and detecting of medicine cationic surfactant.Method for separating and detecting of the present invention is by configuring rationally
The sample solution of concentration, adjusts the running parameter of gas chromatograph, can be prevented effectively from the interference of other compositions in medicine, accurate
Degree is high, reproducible and low cost.
For reaching this purpose, the present invention employs the following technical solutions：
The invention provides a kind of method for separating and detecting of medicine cationic surfactant, methods described includes following
Step：
(1) compounding pharmaceutical sample solution；
(2) the drug sample solution that step (1) is prepared is injected gas chromatograph, molten to drug sample using following condition
Cationic surfactant in liquid carries out separation determination；
Described chromatographic condition is：
Nitrogen buffer gas, control carrier gas flux is 2mL/min～8mL/min, such as 2mL/min, 3mL/min, 4mL/
Min, 5mL/min, 6mL/min, 7mL/min or 8mL/min etc., it is not limited to cited numerical value, in this numerical range
Other unrequited numerical value are equally applicable.
Gas chromatograph injection port temperature is 250 DEG C～300 DEG C, such as 250 DEG C, 260 DEG C, 270 DEG C, 280 DEG C, 290 DEG C
Or 300 DEG C etc., it is not limited to other unrequited numerical value are equally applicable in cited numerical value, this numerical range.
Gas chromatograph column temperature is：Maintain 2min～5min at 90 DEG C～150 DEG C of initial temperature, then with 10 DEG C/min～
The ramp of 15 DEG C/min, to 240 DEG C～260 DEG C, maintains 4min～7min.Wherein, initial temperature can for 90 DEG C, 100 DEG C,
110 DEG C, 120 DEG C, 130 DEG C, 140 DEG C or 150 DEG C etc., it is not limited to cited numerical value, in this numerical range, other are not
The numerical value enumerated is equally applicable；It can be 2min, 3min, 4min or 5min etc. that initial temperature is held time, it is not limited to institute
The numerical value enumerated, in this numerical range, other unrequited numerical value are equally applicable；Heating rate can for 10 DEG C/min, 11 DEG C/
Min, 12 DEG C/min, 13 DEG C/min, 14 DEG C/min or 15 DEG C/min etc., it is not limited to cited numerical value, this numerical value model
In enclosing, other unrequited numerical value are equally applicable；Temperature after intensification can be 240 DEG C, 245 DEG C, 250 DEG C, 255 DEG C or 260 DEG C
Deng it is not limited to other unrequited numerical value are equally applicable in cited numerical value, this numerical range；When maintaining after intensification
Between can be 4min, 5min, 6min or 7min etc., it is not limited to cited numerical value, in this numerical range, other are unrequited
Numerical value equally applicable.
FTD detector temperature be 250 DEG C～320 DEG C, such as 250 DEG C, 260 DEG C, 270 DEG C, 280 DEG C, 290 DEG C, 300 DEG C,
310 DEG C or 320 DEG C etc., it is not limited to other unrequited numerical value are equally applicable in cited numerical value, this numerical range.
Chromatographic condition in gas chromatographic detection separation method of the present invention plays decisive role for testing result,
Wherein carrier gas flux, gas chromatograph injection port temperature and column temperature are both needed to control under certain conditions, just can ensure to test
Accuracy.
In the present invention, described carrier gas flux need to control in 2mL/min～8mL/min, if carrier gas flux is too low, can make mesh
Mark peak retention time is less, separates the accuracy not exclusively reducing test；If carrier gas flux is too high, when target peak can be made to retain
Between larger, detection time is long.
Described injector temperature need to control in 250 DEG C～300 DEG C, if injector temperature is too low, detection signal can be made strong
Spend little, the accuracy of test；If injector temperature is too high, capillary column damaged on end can be made bad.
The initial temperature of described gas chromatograph column temperature need to control in 90 DEG C～150 DEG C, too high can make target peak retain
Time is less, separates the accuracy not exclusively reducing test；Too low can make that target peak retention time is larger, detection time is long.
Likewise, its detection temperature also needs to control in 250 DEG C～320 DEG C, too high capillary column damaged on end can be made bad；Too low can make detection
Signal intensity is little.
Following as currently preferred technical scheme, but the restriction of the technical scheme providing not as the present invention, pass through
Technical scheme below, can preferably reach and realize technical purpose and the beneficial effect of the present invention.
As currently preferred technical scheme, crude drug that described medicine is obtained for fermentation process and its preparation and/or
Crude drug and its preparation that synthetic method is obtained, crude drug and its preparation that preferably fermentation method is obtained, more preferably glass
Glass acid sodium.
Preferably, described preparation is injection.
As currently preferred technical scheme, described cationic surfactant is alkyl quaternaries cation surface
Activating agent.
Preferably, described alkyl quaternaries cation surface active agent is Dodecyl trimethyl ammonium chloride, hexadecane
In base trimethyl ammonium chloride or octadecyl trimethyl ammonium chloride any one or at least two combination, described combination typical case but
Non-limiting examples have：Dodecyl trimethyl ammonium chloride and the combination of hexadecyltrimethylammonium chloride, cetyl front three
Ammonium chloride and the combination of octadecyl trimethyl ammonium chloride, Dodecyl trimethyl ammonium chloride, cetyl trimethyl chlorination
Combination of ammonium and octadecyl trimethyl ammonium chloride etc., preferably hexadecyltrimethylammonium chloride.
As currently preferred technical scheme, the described compounding pharmaceutical sample solution of step (1) is：By medicine and diluent
Be mixed drug sample concentration be 3mg/mL～10mg/mL drug sample solution, such as 3mg/mL, 4mg/mL, 5mg/mL,
6mg/mL, 7mg/mL, 8mg/mL, 9mg/mL or 10mg/mL etc., it is not limited to cited numerical value, in this numerical range
Other unrequited numerical value are equally applicable, and preferably drug sample concentration is the drug sample solution of 5mg/mL.
In the present invention, drug sample concentration also needs to control within the specific limits, if molten excessive concentration, can make target peak response
Value is excessive and so that it is separated not exclusively with other impurities；If concentration is too low can make the too small impact detection of target peak response value accurately
Degree.
Preferably, described diluent is the mixture of second alcohol and water.
Preferably, the mixture of described second alcohol and water is (5～1) for volume ratio:The mixture of (1～5), such as 5:(1～
5)、4:(1～5), 3:(1～5), 2:(1～5) or 1:(1～5) etc., and for example (5～1):1st, (5～1):2nd, (5～1):3rd, (5～
1):4 or (5～1):5 etc., further can 5:1、4:2、3:4、2:3、2:1 or 1:5 etc., it is not limited to cited
Numerical value, in this numerical range, other unrequited numerical value are equally applicable, and preferably volume ratio is 1:1 mixture.
As currently preferred technical scheme, capillary tube in gas chromatograph during the described separation determination of step (2)
Fixative in post is polysiloxanes, preferably methyl polysiloxane.
As currently preferred technical scheme, the logical hydrogen of institute in gas chromatograph during the described separation determination of step (2)
The flow of gas is 20mL/min～50mL/min, such as 20mL/min, 30mL/min, 40mL/min or 50mL/min etc., but simultaneously
It is not limited only to other unrequited numerical value in cited numerical value, this numerical range equally applicable；The flow of institute's blowing air is
200mL/min～500mL/min, such as 200mL/min, 300mL/min, 400mL/min or 500mL/min etc., but and not only
It is limited to other unrequited numerical value in cited numerical value, this numerical range equally applicable.
As currently preferred technical scheme, during the described separation determination of step (2), chromatographic condition is：With nitrogen it is
Carrier gas；Control carrier gas flux is 4mL/min～6mL/min；Gas chromatograph injection port temperature is 275 DEG C～285 DEG C；Gas phase color
Spectrometer column temperature is：Maintain 2min～3min at 115 DEG C～125 DEG C of initial temperature, then the speed with 10 DEG C/min～12 DEG C/min
Rate is warming up to 245 DEG C～255 DEG C, maintains 4min～5min.
Preferably, during the described separation determination of step (2), chromatographic condition is：Nitrogen buffer gas；Control carrier gas flux
For 5mL/min；Gas chromatograph injection port temperature is 280 DEG C；Gas chromatograph column temperature is：Maintain at 120 DEG C of initial temperature
2min, then with the ramp of 10 DEG C/min to 250 DEG C, maintain 4min.
During separation determination in the present invention, chromatographic condition plays decisive role for testing result, and it is again with above-mentioned survey
The result recording under fixed condition is more excellent.
As currently preferred technical scheme, when described medicine is Sodium Hyaluronate, its method for separating and detecting includes following
Step：
(1 ') prepare Sodium Hyaluronate sample solution；
The Sodium Hyaluronate sample solution that step (1 ') is prepared is injected gas chromatograph by (2 '), using following condition to glass
Hexadecyltrimethylammonium chloride in sour sodium sample solution carries out separation determination；
Described chromatographic condition is：
Fixative in capillary column is methyl polysiloxane；
Nitrogen buffer gas, control carrier gas flux is 5mL/min；
Gas chromatograph injection port temperature is 280 DEG C；
Gas chromatograph column temperature is：Maintain 2min at 120 DEG C of initial temperature, then with the ramp of 10 DEG C/min extremely
250 DEG C, maintain 4min；
The temperature of fid detector is 300 DEG C, and the flow of its logical hydrogen of institute is 30mL/min, and the flow of institute's blowing air is
300mL/min.
The present invention for the separation determination of hexadecyltrimethylammonium chloride in medicine Sodium Hyaluronate, with above-mentioned chromatographic condition
The result carrying out separation determination is optimum.
As currently preferred technical scheme, step (1 ') described compounding pharmaceutical sample solution is：By medicine and dilution
Agent is mixed and made into the drug sample solution that drug sample concentration is 5mg/mL.
As currently preferred technical scheme, described diluent is second alcohol and water with volume ratio for 1:The mixing of 1 composition
Thing.
In gas chromatograph used in method for separating and detecting of the present invention, blank solution used is diluent solution, as
The mixture of second alcohol and water, the mixture of described second alcohol and water is (5～1) for volume ratio:The mixture of (1～5), preferably body
Long-pending ratio is 1:1 mixture.
In gas chromatograph, control sample solution used is dissolved in, for cationic surfactant, the solution that diluent is obtained, its
Concentration is 0.001mg/mL～0.01mg/mL, preferably 0.005mg/mL.
Compared with prior art, the invention has the advantages that：
The work ginseng separating the sample solution by reasonable concentration for the method for testing, optimizing gas chromatograph of the present invention
Number, can be prevented effectively from the interference that other constituents in medicine separate test for cationic surfactant, and then can be by
Cationic surfactant is effectively separated from medicine, and accurately calculates containing of medicine cationic surfactant
Amount, up to 100%, precision is high, reproducible for its response rate.And gas chromatograph used is compared with other test instrunments, valency
Lattice are cheap, and cost is lower.
Brief description
Fig. 1 is linear test color spectrogram in the embodiment of the present invention 1；
Fig. 2 is the linearity curve of linear test in the embodiment of the present invention 1.
Specific embodiment
For the present invention is better described, readily appreciate technical scheme, below to the present invention further specifically
Bright.But following embodiments is only the simple example of the present invention, does not represent or limit the scope of the present invention, this
Invention protection domain is defined by claims.
Specific embodiment of the invention part provides a kind of method for separating and detecting of medicine cationic surfactant, institute
The method of stating comprises the following steps：
(1) compounding pharmaceutical sample solution；
(2) the drug sample solution that step (1) is prepared is injected gas chromatograph, molten to drug sample using following condition
Cationic surfactant in liquid carries out separation determination；
Described chromatographic condition is：
Nitrogen buffer gas, control carrier gas flux is 2mL/min～8mL/min；
Gas chromatograph injection port temperature is 250 DEG C～300 DEG C；
Gas chromatograph column temperature is：Maintain 2min～5min at 90 DEG C～150 DEG C of initial temperature, then with 10 DEG C/min～
The ramp of 15 DEG C/min, to 240 DEG C～260 DEG C, maintains 4min～7min.
FTD detector temperature is 250 DEG C～320 DEG C.
It is below present invention typical case but non-limiting example：
Embodiment 1：
Present embodiments provide cetyl trimethyl chlorination in a kind of Sodium Hyaluronate of fermentation technology production and its preparation
The method of separating and assaying of ammonium：
In this method of separating and assaying, blank solution used is diluent, and that is, ethanol and water are with volume ratio 50:50 preparations obtain；
Being formulated as of reference substance solution used：
Weigh hexadecyltrimethylammonium chloride 25mg and be placed in 50mL volumetric flask, plus diluent dissolves and is diluted to scale,
Shake up, then pipette 0.1mL and be placed in another 10ml volumetric flask, be diluted to scale with diluent, shake up, molten as reference substance
Liquid.
Drug sample solution used is：
Take sample about 50mg, accurately weighed, it is placed in 10mL volumetric flask, plus diluent 5mL, vibrate 5 minutes, plus diluent is dilute
Release to scale, shake up, stand 15min, take solution centrifugal 15min, take supernatant solution, as drug sample solution.
The drug sample solution that step is prepared injects gas chromatograph, using following condition in drug sample solution
Cationic surfactant carries out separation determination；
Fixative in capillary column is methyl polysiloxane；
Nitrogen is carrier gas, and control carrier gas flux is 5mL/min；
Gas chromatograph injection port temperature is 280 DEG C；
Gas chromatograph column temperature is：Maintain 2min at 120 DEG C of initial temperature, then with the ramp of 10 DEG C/min extremely
250 DEG C, maintain 4min.
The temperature of fid detector is 300 DEG C, and the flow of its logical hydrogen of institute is 30mL/min, and the flow of institute's blowing air is
300mL/min.
Capillary column used is Agilent 30m*0.32mm, 0.5um；Described gas chromatograph is Agilent7890A.
Precision measures blank solution, reference substance solution and the drug sample solution of the above-mentioned preparation of 1 μ L respectively, injects gas phase color
Spectrometer (INSTRUMENT MODEL：), and record chromatogram Agilent7890A.
With the content of hexadecyltrimethylammonium chloride in external standard method drug sample solution, the results detailed in Table 1.
Table 1：Hexadecyltrimethylammonium chloride content detection analytical table in drug sample solution
Note：NA represents inapplicable.
From table 1 it follows that this method can make the cationic surfactant ten in reference substance solution and sample solution
Six alkyl trimethyl ammonium chlorides reach fine separation, and accurately calculate cetyl trimethyl chlorine in mensure drug sample solution
Change the content of ammonium, up to 100%, precision is high for its response rate, and repeatability is good.
Linearity curve is tested：
The preparation of linear test solution：Weigh hexadecyltrimethylammonium chloride 25mg and be placed in 50mL volumetric flask, plus dilution
Agent is dissolved and is diluted to scale, shakes up, then pipette from three volumetric flasks respectively 0.6mL, 0.4mL, 0.2mL, 0.1mL,
0.05mL and 0.025mL is respectively placed in 10mL volumetric flask, is diluted to scale with diluent, shakes up, right as 6 variable concentrations
According to product linear solvent.
Precision measures the reference substance linear solvent of 6 variable concentrations of the above-mentioned preparation of 1 μ L respectively, injects gas chromatograph,
And adopt above-mentioned GC conditions, and record chromatogram (as shown in Figure 1).
Calculate the peak area recording, result is as shown in table 2.And linearly divided according to the peak area recording and actual concentrations
Analysis, and draw linearity curve (as shown in Figure 2).
Table 2：Linear test data result table
From the result of table 2 and Fig. 1 and Fig. 2 can be seen that the present invention offer gas chromatography to sample middle-jiao yang, function of the spleen and stomach from
The separation determination of sublist face lammonium ammonium chloride, hexadecyltrimethylammonium chloride concentration be 1.02～
There is in the range of 30.72ug/mL good linear relationship with peak area.
Embodiment 2：
Present embodiments provide cetyl trimethyl chlorination in a kind of Sodium Hyaluronate of fermentation technology production and its preparation
The method of separating and assaying of ammonium：
In this method of separating and assaying, blank solution used is diluent, and that is, ethanol and water are with volume ratio 50:50 preparations obtain；
Being formulated as of reference substance solution used：
Weigh hexadecyltrimethylammonium chloride 25mg and be placed in 50mL volumetric flask, plus diluent dissolves and is diluted to scale,
Shake up, then pipette 0.1mL and be placed in another 10ml volumetric flask, be diluted to scale with diluent, shake up, molten as reference substance
Liquid.
Drug sample solution used is：
Take sample about 50mg, accurately weighed, it is placed in 10mL volumetric flask, plus diluent 5mL, vibrate 5 minutes, plus diluent is dilute
Release to scale, shake up, stand 15min, take solution centrifugal 15min, take supernatant solution, as drug sample solution.
The drug sample solution that step is prepared injects gas chromatograph, using following condition in drug sample solution
Cationic surfactant carries out separation determination；
Fixative in capillary column is polysiloxanes；
Nitrogen is carrier gas, and control carrier gas flux is 4mL/min；
Gas chromatograph injection port temperature is 275 DEG C；
Gas chromatograph column temperature is：Maintain 3min at 115 DEG C of initial temperature, then with the ramp of 12 DEG C/min extremely
245 DEG C, maintain 5min；
The temperature of fid detector is 290 DEG C, and the flow of its logical hydrogen of institute is 25mL/min, and the flow of institute's blowing air is
250mL/min.
Capillary column used is Agilent 30m*0.32mm, 0.5um；Described gas chromatograph is Agilent7890A.
Precision measures blank solution, reference substance solution and the drug sample solution of the above-mentioned preparation of 1 μ L respectively, injects gas phase color
Spectrometer, and record chromatogram.
With in external standard method drug sample solution, the content of hexadecyltrimethylammonium chloride is for 0.00301%, its time
, up to 100.3%, precision is high for yield, and repeatability is good.
Embodiment 3：
Present embodiments provide Dodecyl trimethyl ammonium chloride in a kind of medicine of fermentation technology production and its preparation
Method of separating and assaying：
Being formulated as of reference substance solution used：
Weigh Dodecyl trimethyl ammonium chloride 25mg and be placed in 50mL volumetric flask, plus diluent dissolves and is diluted to scale,
Shake up, then pipette 0.1mL and be placed in another 10ml volumetric flask, be diluted to scale with diluent, shake up, molten as reference substance
Liquid.
Drug sample solution used is：
Take sample about 50mg, accurately weighed, it is placed in 10mL volumetric flask, plus diluent 5mL, vibrate 5 minutes, plus diluent is dilute
Release to scale, shake up, stand 15min, take solution centrifugal 15min, take supernatant solution, as drug sample solution.
The drug sample solution that step is prepared injects gas chromatograph, using following condition in drug sample solution
Cationic surfactant carries out separation determination；
Fixative in capillary column is polysiloxanes；
Nitrogen is carrier gas, and control carrier gas flux is 6mL/min；
Gas chromatograph injection port temperature is 285 DEG C；
Gas chromatograph column temperature is：Maintain 4min at 125 DEG C of initial temperature, then with the ramp of 15 DEG C/min extremely
255 DEG C, maintain 5min；
The temperature of fid detector is 310 DEG C, and the flow of its logical hydrogen of institute is 35mL/min, and the flow of institute's blowing air is
350mL/min.
Capillary column used is Agilent 30m*0.32mm, 0.5um；Described gas chromatograph is Agilent 7890A.
Precision measures blank solution, reference substance solution and the drug sample solution of the above-mentioned preparation of 1 μ L respectively, injects gas phase color
Spectrometer, and record chromatogram.
With in external standard method drug sample solution, the content of Dodecyl trimethyl ammonium chloride is for 0.00303%, its time
, up to 100.3%, precision is high for yield, and repeatability is good.
Embodiment 4：
Present embodiments provide octadecyl trimethyl ammonium chloride in a kind of medicine of fermentation technology production and its preparation
Method of separating and assaying, methods described except the condition of gas chromatograph is：Fixative in capillary column is methyl polysiloxane；
Nitrogen is carrier gas, and control carrier gas flux is 2mL/min；
Gas chromatograph injection port temperature is 250 DEG C；
Gas chromatograph column temperature is：Maintain 5min at 90 DEG C of initial temperature, then with the ramp of 10 DEG C/min to 240
DEG C, maintain 7min.
The temperature of fid detector is 250 DEG C, and the flow of its logical hydrogen of institute is 20mL/min, and the flow of institute's blowing air is
200mL/min.
Capillary column used is Agilent 30m*0.32mm, 0.5um；Described gas chromatograph is Agilent 7890A.
Other processes are all in the same manner as in Example 1, with octadecyl trimethyl chlorine in external standard method drug sample solution
The content changing ammonium is 0.00302%, and, up to 100.7%, precision is high for its response rate, and repeatability is good.
Embodiment 5：
Present embodiments provide hexadecyltrimethylammonium chloride in a kind of medicine of fermentation technology production and its preparation
Method of separating and assaying, methods described except the condition of gas chromatograph is：Fixative in capillary column is methyl polysiloxane；
Nitrogen is carrier gas, and control carrier gas flux is 8mL/min；
Gas chromatograph injection port temperature is 300 DEG C；
Gas chromatograph column temperature is：Maintain 2min at 150 DEG C of initial temperature, then with the ramp of 10 DEG C/min extremely
260 DEG C, maintain 4min；
The temperature of fid detector is 320 DEG C, and the flow of its logical hydrogen of institute is 50mL/min, and the flow of institute's blowing air is
500mL/min.
Other processes are all in the same manner as in Example 1, with cetyl trimethyl chlorine in external standard method drug sample solution
The content changing ammonium is 0.00301%, and, up to 100.3%, precision is high for its response rate, and repeatability is good.
Comparative example 1：
This comparative example provides hexadecyltrimethylammonium chloride in a kind of medicine of fermentation technology production and its preparation
Method of separating and assaying, methods described except in the condition of gas chromatograph carrier gas flux be 15mL/min (＞ 8mL/min) in addition to, its
His process is all in the same manner as in Example 1, with the content of hexadecyltrimethylammonium chloride in external standard method drug sample solution
For 0.00415%, its accuracy rate is only 138.3%, and precision is poor.
Comparative example 2：
This comparative example provides hexadecyltrimethylammonium chloride in a kind of medicine of fermentation technology production and its preparation
Method of separating and assaying, methods described except gas chromatograph injection port temperature be 180 DEG C (250 DEG C of ＜) in addition to, other processes all with
Identical in embodiment 1, the content with hexadecyltrimethylammonium chloride in external standard method drug sample solution is
0.00233%, its response rate is only 77.7%, and precision is poor.
Comparative example 3：
This comparative example provides hexadecyltrimethylammonium chloride in a kind of medicine of fermentation technology production and its preparation
Method of separating and assaying, methods described except gas chromatograph injection port temperature be 350 DEG C (300 DEG C of ＞) in addition to, other processes all with
Identical in embodiment 1, the content with hexadecyltrimethylammonium chloride in external standard method drug sample solution is
0.00432%, its response rate is only 144.0%, and precision is poor.
Comparative example 4：
This comparative example provides hexadecyltrimethylammonium chloride in a kind of medicine of fermentation technology production and its preparation
Method of separating and assaying, methods described except gas chromatograph column temperature initial temperature be 60 DEG C (90 DEG C of ＜) in addition to, other processes all with
Identical in embodiment 1, the content with hexadecyltrimethylammonium chloride in external standard method drug sample solution is
0.00227%, its response rate is only 75.7%, and precision is poor.
Comparative example 5：
This comparative example provides hexadecyltrimethylammonium chloride in a kind of medicine of fermentation technology production and its preparation
Method of separating and assaying, in addition to gas chromatograph column temperature initial temperature is 200 DEG C (150 DEG C of ＞), other processes are equal for methods described
In the same manner as in Example 1, the content with hexadecyltrimethylammonium chloride in external standard method drug sample solution is
0.00251%, its response rate is only 83.7%, and precision is poor.
Comparative example 6：
This comparative example provides hexadecyltrimethylammonium chloride in a kind of medicine of fermentation technology production and its preparation
Method of separating and assaying, in addition to gas chromatograph column temperature final temperature temperature is 150 DEG C (240 DEG C of ＜), other processes are equal for methods described
In the same manner as in Example 1, the content with hexadecyltrimethylammonium chloride in external standard method drug sample solution is
0.00231%, its response rate is only 77.0%, and precision is poor.
Comparative example 7：
This comparative example provides hexadecyltrimethylammonium chloride in a kind of medicine of fermentation technology production and its preparation
Method of separating and assaying, in addition to gas chromatograph column temperature final temperature temperature is 300 DEG C (260 DEG C of ＞), other processes are equal for methods described
In the same manner as in Example 1, the content with hexadecyltrimethylammonium chloride in external standard method drug sample solution is
0.00219%, its response rate is only 73.0%, and precision is poor.
The result of integrated embodiment 1-5 and comparative example 1-6 can be seen that the method for testing that separates of the present invention and passes through rationally
The sample solution of concentration, optimizes the running parameter of gas chromatograph, can be prevented effectively from medicine other constituents for sun from
Sub- surfactant separates the interference of test, and then effectively can separate cationic surfactant from medicine,
And accurately calculating the content of medicine cationic surfactant, up to 100%, precision is high, reproducible for its response rate.And
Gas chromatograph used is compared with other test instrunments, cheap, and cost is lower.
Applicant states, the present invention illustrates the method detailed of the present invention by above-described embodiment, but the present invention not office
It is limited to above-mentioned method detailed, that is, do not mean that the present invention has to rely on above-mentioned method detailed and could implement.Art
Technical staff is it will be clearly understood that any improvement in the present invention, the equivalence replacement to each raw material of product of the present invention and auxiliary element
Interpolation, selection of concrete mode etc., within the scope of all falling within protection scope of the present invention and disclosure.
Claims (10)
1. a kind of method for separating and detecting of medicine cationic surfactant is it is characterised in that methods described includes following step
Suddenly：
(1) compounding pharmaceutical sample solution；
(2) the drug sample solution that step (1) is prepared is injected gas chromatograph, using following condition in drug sample solution
Cationic surfactant carry out separation determination；
Described chromatographic condition is：
Nitrogen buffer gas, control carrier gas flux is 2mL/min～8mL/min；
Gas chromatograph injection port temperature is 250 DEG C～300 DEG C；
Gas chromatograph column temperature is：Maintain 2min～5min at 90 DEG C～150 DEG C of initial temperature, then with 10 DEG C/min～15
DEG C/ramp of min to 240 DEG C～260 DEG C, maintain 4min～7min；
FTD detector temperature is 250 DEG C～320 DEG C.
2. the method for separating and detecting according to claim 1 it is characterised in that described medicine for fermentation process be obtained former
Crude drug and its preparation that material medicine and its preparation and/or synthetic method are obtained, crude drug and its system that preferably fermentation method is obtained
Agent, more preferably Sodium Hyaluronate；
Preferably, described preparation is injection.
3. method for separating and detecting according to claim 1 and 2 is it is characterised in that described cationic surfactant is alkane
Based quaternary ammonium salt cationoid surfactant；
Preferably, described alkyl quaternaries cation surface active agent is Dodecyl trimethyl ammonium chloride, cetyl three
In ammonio methacrylate or octadecyl trimethyl ammonium chloride any one or at least two combination, preferably cetyl front three
Ammonium chloride.
4. the method for separating and detecting according to any one of claim 1-3 is it is characterised in that the described compounding pharmaceutical of step (1)
Sample solution is：Medicine and diluent are mixed and made into the drug sample solution that drug sample concentration is 3mg/mL～10mg/mL,
It is preferably the drug sample solution that drug sample concentration is 5mg/mL；
Preferably, described diluent is the mixture of second alcohol and water；
Preferably, the mixture of described second alcohol and water is (5～1) for volume ratio:The mixture of (1～5), preferably volume ratio are
1:1 mixture.
5. the method for separating and detecting according to any one of claim 1-4 is it is characterised in that the described separation determination of step (2)
During fixative in capillary column in gas chromatograph be polysiloxanes, preferably methyl polysiloxane.
6. the method for separating and detecting according to any one of claim 1-5 is it is characterised in that the described separation determination of step (2)
During in gas chromatograph fid detector the flow of logical hydrogen be 20mL/min～50mL/min, the flow of institute's blowing air
For 200mL/min～500mL/min；
Preferably, the temperature of described fid detector be 290～310 DEG C, its institute logical hydrogen flow be 25mL/min～35mL/
Min, the flow of institute's blowing air is 250mL/min～350mL/min, and the more preferably temperature of fid detector is 300 DEG C,
Its flow of logical hydrogen be 30mL/min, the flow of institute's blowing air is 300mL/min.
7. the method for separating and detecting according to any one of claim 1-6 is it is characterised in that the described separation determination of step (2)
During chromatographic condition be：Nitrogen buffer gas；Control carrier gas flux is 4mL/min～6mL/min；Gas chromatograph injection port
Temperature is 275 DEG C～285 DEG C；Gas chromatograph column temperature is：Maintain 2min～3min at 115 DEG C～125 DEG C of initial temperature, then
With the ramp of 10 DEG C/min～12 DEG C/min to 245 DEG C～255 DEG C, maintain 4min～5min；
Preferably, chromatographic condition during the described separation determination of step (2)：Nitrogen buffer gas；Control carrier gas flux is 5mL/
min；Gas chromatograph injection port temperature is 280 DEG C；Gas chromatograph column temperature is：Maintain 2min at 120 DEG C of initial temperature, then
With the ramp of 10 DEG C/min to 250 DEG C, maintain 4min.
8. the method for separating and detecting according to any one of claim 1-7 is it is characterised in that described medicine is Sodium Hyaluronate
When, its method for separating and detecting comprises the following steps：
(1 ') prepare Sodium Hyaluronate sample solution；
The Sodium Hyaluronate sample solution that step (1 ') is prepared is injected gas chromatograph by (2 '), using following condition to Sodium Hyaluronate
Hexadecyltrimethylammonium chloride in sample solution carries out separation determination；
Described chromatographic condition is：
Fixative in capillary column is methyl polysiloxane；
Nitrogen buffer gas, control carrier gas flux is 5mL/min；
Gas chromatograph injection port temperature is 280 DEG C；
Gas chromatograph column temperature is：Maintain 2min at 120 DEG C of initial temperature, then with the ramp of 10 DEG C/min to 250 DEG C,
Maintain 4min；
The temperature of fid detector is 300 DEG C, and the flow of its logical hydrogen of institute is 30mL/min, and the flow of institute's blowing air is 300mL/
min.
9. method for separating and detecting according to claim 8 is it is characterised in that step (1 ') described compounding pharmaceutical sample solution
For：Medicine and diluent are mixed and made into the drug sample solution that drug sample concentration is 5mg/mL.
10. method for separating and detecting according to claim 9 is it is characterised in that described diluent is second alcohol and water with volume
Than for 1:The mixture of 1 composition.
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| CN112345659A (en) * | 2020-09-25 | 2021-02-09 | 安徽省公众检验研究院有限公司 | Gas chromatography analysis method for detecting content of decamethyl ammonium bromide |
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