CN106153749A - The method of residual solvent in inspection chlophedianol hydrochloride Starting material medicine - Google Patents
The method of residual solvent in inspection chlophedianol hydrochloride Starting material medicine Download PDFInfo
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Abstract
The present invention relates to a kind of check the method for residual solvent in chlophedianol hydrochloride Starting material medicine.The capillary column (DB-624,0.53 mm × 30m, 3.0 μm) using 6% cyanogen propyl group phenyl-94% dimethyl polysiloxane to be fixative, temperature programming, initial temperature 40 DEG C, keep 3min, with the ramp of 20 DEG C/min to 240 DEG C, keep 3min；Flame ionization ditector (FID), detector temperature 250 DEG C, injector temperature 200 DEG C, carrier gas is helium, flow velocity 5mL/min, sampling volume 1mL.Split ratio 1:1.5 kinds of organic solvent (methanol, ethanol, acetonitrile, benzene, toluene) sample introduction concentration are good linear relation with peak area as a result, and correlation coefficient is all higher than 0.9990, and average recovery is between 96.0% ~ 103.0%；Advantage is to improve rationally, accurately and reliably, highly sensitive, can be used for the mensuration of residual solvent in chlophedianol.
Description
Technical field
The present invention relates in chlophedianol hydrochloride Starting material medicine residual solvent inspection field, be specifically related to a kind of check the method for residual solvent in chlophedianol hydrochloride Starting material medicine.
Background technology
Chlophedianol in addition to having central antitussive effect, also antihistaminic effect and atropine-like effect, bronchospasm and mucous hyperemia edema can be alleviated.It is applicable to dry cough or apasm of coughing that respiratory tract actute infection causes, often share with expectorant.Solvent in the building-up process of chlophedianol has benzene, toluene, methanol, ethanol, acetonitrile, these solvents inevitably remain in finished product, according to Chinese Pharmacopoeia and ICH regulation limited to dissolvent residual, but method residual solvent in chlophedianol tested currently without a kind of the most perfect method.
Summary of the invention
In order to solve the problems referred to above, the present invention proposes and a kind of checks the method for residual solvent in chlophedianol hydrochloride Starting material medicine, and method is improved rationally, accurately and reliably, highly sensitive, can be used for the mensuration of residual solvent in chlophedianol.
In order to reach foregoing invention purpose, the present invention proposes techniques below scheme:
The method of residual solvent in inspection chlophedianol hydrochloride Starting material medicine, it is characterised in that following steps,
1) prepared by solution
Prepared by comparison stock solution: precision weighs acetonitrile 205mg, toluene 445mg, absolute methanol 1500mg, dehydrated alcohol 2500mg, benzole soln (1mg/ml) 1.0ml, is placed in 100ml volumetric flask, is diluted to scale with DMF aqueous solution (10 → 100), shakes up；
Prepared by contrast solution: precision pipette 1.0ml comparison stock solution in 100ml volumetric flask, add DMF aqueous solution (10 → 100), be diluted to scale, shake up and get final product, precision pipettes 10.0ml and is placed in ml headspace bottle；
Prepared by need testing solution: take chlophedianol about 0.5g, accurately weighed, adds DMF aqueous solution (10 → 100) 10mL, dissolves, as need testing solution；
2) chromatographic condition
DB-624 capillary column, fid detector, detector temperature 250 DEG C, injector temperature 200 DEG C；Carrier gas is helium, purity 99.99%, flow velocity 5mL/min；Use temperature programming, initial temperature 40 DEG C, keep 3min, with the ramp of 20 DEG C/min to 240 DEG C, keep 3min；Ml headspace bottle equilibrium temperature 80 DEG C, equilibration time 25min, sample size 1mL；Quantitative loop temperature 120 DEG C, transmission line temperature 130 DEG C；Split ratio 1:1；
3) system suitability and precision test
Record chromatogram, five kinds of solvent separating degrees are good, and empirical tests peak sequence is methanol, ethanol, acetonitrile, benzene, toluene；Separating degree between each peak is followed successively by 2.2,10.6,10.6,12.0,8.1, and separating degree is all higher than 1.5, and chromatographic peak is kept completely separate；The relative standard deviation (RSD) of its peak area is respectively 4.4%, 4.5%, 3.7%, 2.5%, 8.1%, and the relative standard deviation (RSD) of peak retention time is respectively 0.02%, 0.01%, 0.01%, 0.01%, 0.02%；
4) linear relationship and detection limit test
Precision measures reference substance stock solution 200 μ l respectively, 150 μ l, 100 μ l, 50 μ l, 10 μ l, 5 μ l, are placed in headspace sampling bottle, then precision measures 10mL DMF aqueous solution (10 → 100) respectively, mixing, by the 2nd) chromatographic condition sample introduction under item, record chromatogram, with concentration (C), peak area (A) is carried out linear regression；
Reducing concentration by stepwise dilution, sample introduction measures, and records detection limit respectively 0.171,0.425,0.0699,0.0127, the 0.00585 μ g/mL of methanol, ethanol, acetonitrile, benzene, toluene, the content being converted in sample is respectively 3.4ppm, 8.5ppm, 1.4ppm, 0.03ppm, 0.12ppm；
5) response rate
The most each preparation measures the 50% of limit, 100%, 150% sample solution adding contrast solution, by the 2nd) chromatographic condition under item, calculate by external standard method, methanol, ethanol, acetonitrile, benzene, toluene average recovery rate are respectively 98.8%, 99.6%, 100.7%, 101.8%, 100.5%, and RSD is respectively 5.3%, 6.5%, 2.8%, 9.4%, 7.2%；
6) replica test
Take with a collection of test sample, totally six parts, by the 1st) method of item prepares need testing solution, by the 2nd) chromatographic condition sample introduction, record chromatogram, calculate methanol in sample by external standard method, ethanol, acetonitrile, benzene, the residual quantity of toluene are respectively 290ppm, 89ppm, do not detect, do not detect, 5ppm, RSD are respectively 5.6%, 4.2%, do not detect, do not detect, 5.7%；
Take chlophedianol three batches, by the 1st) method of item prepares need testing solution, by the 2nd) chromatographic condition sample introduction, record chromatogram, calculate the residual quantity of each solvent in sample by external standard method.
Capillary column (DB-624,0.53 mm × 30 that described capillary column uses 6 % cyanogen propyl group phenyl-94 % dimethyl polysiloxanes to be fixative
M, 3.0 μm).
It is an advantage of the invention that the capillary column (DB-624,0.53 mm × 30 m, 3.0 μm) using 6 % cyanogen propyl group phenyl-94 % dimethyl polysiloxanes to be fixative, temperature programming, initial temperature 40 DEG C, keep 3
Min, with the ramp of 20 DEG C/min to 240 DEG C, keeps 3 min；Flame ionization ditector (FID), detector temperature 250 DEG C, injector temperature 200 DEG C, carrier gas is helium, flow velocity 5 mL/min, sampling volume 1 mL.Split ratio 1:1.5 kinds of organic solvent (methanol, ethanol, acetonitrile, benzene, toluene) sample introduction concentration are good linear relation with peak area as a result, and correlation coefficient is all higher than 0.9990, and average recovery is between 96.0 % ~ 103.0 %；This method is improved rationally, accurately and reliably, highly sensitive, can be used for the mensuration of residual solvent in chlophedianol.
Accompanying drawing explanation
The separating degree chromatogram schematic diagram of Fig. 1 present invention.
Detailed description of the invention
1 instrument and reagent
Agilent 7890N gas chromatograph (U.S.'s Agilent)；Agilent 7694E head-space sampler (U.S.'s Agilent)；Capillary column: DB-624(30m × 0.53mm, 3.0 μm)；Benzene, toluene, absolute methanol, ethanol, acetonitrile are analytical pure, and DMF is chromatographically pure；Chlophedianol (Jiangsu Baozong Baoda Pharmaceutical Co., Ltd., lot number: 1041210001,1041210002,1041210003).
2 methods and result
Prepared by 2.1 solution
Prepared by comparison stock solution: precision weighs acetonitrile 205mg, toluene 445mg, absolute methanol 1500mg, dehydrated alcohol 2500mg, benzole soln (1mg/ml) 1.0ml, is placed in 100ml volumetric flask, is diluted to scale with DMF aqueous solution (10 → 100), shakes up.
Prepared by contrast solution: precision pipette 1.0ml comparison stock solution in 100ml volumetric flask, add DMF aqueous solution (10 → 100), be diluted to scale, shake up and get final product, precision pipettes 10.0ml and is placed in ml headspace bottle.
Prepared by need testing solution: take chlophedianol about 0.5g, accurately weighed, adds DMF aqueous solution (10 → 100) 10mL, dissolves, as need testing solution.
2.2 chromatographic condition
DB-624 capillary column, fid detector, detector temperature 250 DEG C, injector temperature 200 DEG C；Carrier gas is helium, purity 99.99%, flow velocity
5mL/min；Use temperature programming, initial temperature 40 DEG C, keep 3min, with the ramp of 20 DEG C/min to 240 DEG C, keep 3min；Ml headspace bottle equilibrium temperature 80 DEG C, equilibration time 25min, sample size 1mL；Quantitative loop temperature 120 DEG C, transmission line temperature 130 DEG C
2.3 system suitabilitys and precision test
Record chromatogram, 5 kinds of solvent separating degrees are good, see that Fig. 1, empirical tests peak sequence are methanol, ethanol, acetonitrile, benzene, toluene；Separating degree between each peak is followed successively by 2.2,10.6,10.6,12.0,8.1, and separating degree is all higher than 1.5, and chromatographic peak is kept completely separate；The relative standard deviation (RSD) of its peak area is respectively 4.4%, 4.5%, 3.7%, 2.5%, 8.1%, the relative standard deviation (RSD) of peak retention time is respectively 0.02%, 0.01%, 0.01%, 0.01%, 0.02%, show that instrument precision is good, method favorable reproducibility.It can be seen that 1: methanol (2.4min) 2: ethanol (3.3min) 3: acetonitrile (4.0min) 4: benzene (6.1min) 5: toluene (7.4min).
2.4 linear relationships and detection limit test
Precision measures reference substance stock solution 200 μ l, 150 μ l, 100 μ l respectively, 50 μ l, 10 μ l, 5 μ l, be placed in headspace sampling bottle, precision measures 10mL DMF aqueous solution (10 → 100) the most respectively, mixing, by the chromatographic condition sample introduction under 2.2, records chromatogram, with concentration (C), peak area (A) is carried out linear regression, the results are shown in Table 1.
Table 1 equation of linear regression and range of linearity measurement result
| Solvent | Regression equation | The range of linearity/mg.mL-1 | Correlation coefficient |
| Methanol | Y=696.5X-0.3936 | 0.007534~0.30134 | 0.9999 |
| Ethanol | Y=1375.7X-0.8374 | 0.01245~0.4983 | 0.9998 |
| Acetonitrile | Y=62285.2X-0.6655 | 0.001002~0.04008 | 0.9997 |
| Benzene | Y=80352.4X-0.0805 | 0.0000575~0.0023 | 0.9990 |
| Toluene | Y=74789.9X-50.6322 | 0.002247~0.08986 | 0.9991 |
Reducing concentration by stepwise dilution, sample introduction measures, and records detection limit respectively 0.171,0.425,0.0699,0.0127, the 0.00585 μ g/mL of methanol, ethanol, acetonitrile, benzene, toluene, the content being converted in sample is respectively 3.4ppm, 8.5ppm, 1.4ppm, 0.03ppm, 0.12ppm..
2.5 the response rate
The most each preparation measures the 50% of limit, 100%, 150% sample solution adding contrast solution, by the chromatographic condition under 2.2, calculate by external standard method, methanol, ethanol, acetonitrile, benzene, toluene average recovery rate are respectively 98.8%, 99.6%, 100.7%, 101.8%, 100.5%, and RSD is respectively 5.3%, 6.5%, 2.8%, 9.4%, 7.2%.
2.6 replica test
Take with a collection of test sample (lot number: 1041210001), totally 6 parts, need testing solution is prepared by the method for 2.1, by 2.2 chromatographic condition sample introductions, record chromatogram, calculate methanol in sample by external standard method, ethanol, acetonitrile, benzene, the residual quantity of toluene are respectively 290ppm, 89ppm, do not detect, do not detect, 5ppm, RSD are respectively 5.6%, 4.2%, do not detect, do not detect, 5.7%.
2.7 sample determination
Take chlophedianol 3 batches (lot number: 1041210001,1041210002,1041210003), prepare need testing solution by the method for 2.1, by 2.2 chromatographic condition sample introductions, record chromatogram, calculating the residual quantity of each solvent in sample by external standard method, the measurement result of 3 batch samples is shown in Table 2.
Table 2
Sample determination result
| Solvent | 1041210001 | 1041210002 | 1041210003 |
| Methanol | 290ppm | 374ppm | 323ppm |
| Ethanol | 89ppm | 136ppm | 98ppm |
| Acetonitrile | Do not detect | Do not detect | Do not detect |
| Benzene | Do not detect | Do not detect | Do not detect |
| Toluene | 5ppm | 0.2ppm | 0.2ppm |
3 discuss
The selection of 3.1 equilibrium temperatures
The highest equilibrium temperature can improve sensitivity, reduces equilibration time, but test sample and residual solvent can be caused to decompose or occur other to change by high-temperature, also can cause the problems such as the pressure of head space and air-tightness, increase analytical error.Prerun series of temperature herein, 80 DEG C of ratios are conveniently.
The selection of 3.2 equilibration times
Having investigated 20, the different equilibration time impacts on result such as 25,30,40min, after indicating 30min, peak area the most no longer increases, therefore selecting 30min is equilibration time.
Claims (2)
1. the method for residual solvent in inspection chlophedianol hydrochloride Starting material medicine, it is characterised in that following steps,
1) prepared by solution
Prepared by comparison stock solution: precision weighs acetonitrile 205mg, toluene 445mg, absolute methanol 1500mg, dehydrated alcohol 2500mg, benzole soln (1mg/ml) 1.0ml, is placed in 100ml volumetric flask, is diluted to scale with DMF aqueous solution (10 → 100), shakes up；
Prepared by contrast solution: precision pipette 1.0ml comparison stock solution in 100ml volumetric flask, add DMF aqueous solution (10 → 100), be diluted to scale, shake up and get final product, precision pipettes 10.0ml and is placed in ml headspace bottle；
Prepared by need testing solution: take chlophedianol about 0.5g, accurately weighed, adds DMF aqueous solution (10 → 100) 10mL, dissolves, as need testing solution；
2) chromatographic condition
DB-624 capillary column, fid detector, detector temperature 250 DEG C, injector temperature 200 DEG C；Carrier gas is helium, purity 99.99%, flow velocity 5mL/min；Use temperature programming, initial temperature 40 DEG C, keep 3min, with the ramp of 20 DEG C/min to 240 DEG C, keep 3min；Ml headspace bottle equilibrium temperature 80 DEG C, equilibration time 25min, sample size 1mL；Quantitative loop temperature 120 DEG C, transmission line temperature 130 DEG C；Split ratio 1:1；
3) system suitability and precision test
Record chromatogram, five kinds of solvent separating degrees are good, and empirical tests peak sequence is methanol, ethanol, acetonitrile, benzene, toluene；Separating degree between each peak is followed successively by 2.2,10.6,10.6,12.0,8.1, and separating degree is all higher than 1.5, and chromatographic peak is kept completely separate；The relative standard deviation (RSD) of its peak area is respectively 4.4%, 4.5%, 3.7%, 2.5%, 8.1%, and the relative standard deviation (RSD) of peak retention time is respectively 0.02%, 0.01%, 0.01%, 0.01%, 0.02%；
4) linear relationship and detection limit test
Precision measures reference substance stock solution 200 μ l respectively, 150 μ l, 100 μ l, 50 μ l, 10 μ l, 5 μ l, are placed in headspace sampling bottle, then precision measures 10mL DMF aqueous solution (10 → 100) respectively, mixing, by the 2nd) chromatographic condition sample introduction under item, record chromatogram, with concentration (C), peak area (A) is carried out linear regression；
Reducing concentration by stepwise dilution, sample introduction measures, and records detection limit respectively 0.171,0.425,0.0699,0.0127, the 0.00585 μ g/mL of methanol, ethanol, acetonitrile, benzene, toluene, the content being converted in sample is respectively 3.4ppm, 8.5ppm, 1.4ppm, 0.03ppm, 0.12ppm；
5) response rate
The most each preparation measures the 50% of limit, 100%, 150% sample solution adding contrast solution, by the 2nd) chromatographic condition under item, calculate by external standard method, methanol, ethanol, acetonitrile, benzene, toluene average recovery rate are respectively 98.8%, 99.6%, 100.7%, 101.8%, 100.5%, and RSD is respectively 5.3%, 6.5%, 2.8%, 9.4%, 7.2%；
6) replica test
Take with a collection of test sample, totally six parts, by the 1st) method of item prepares need testing solution, by the 2nd) chromatographic condition sample introduction, record chromatogram, calculate methanol in sample by external standard method, ethanol, acetonitrile, benzene, the residual quantity of toluene are respectively 290ppm, 89ppm, do not detect, do not detect, 5ppm, RSD are respectively 5.6%, 4.2%, do not detect, do not detect, 5.7%；
Take chlophedianol three batches, by the 1st) method of item prepares need testing solution, by the 2nd) chromatographic condition sample introduction, record chromatogram, calculate the residual quantity of each solvent in sample by external standard method.
The method of residual solvent in inspection chlophedianol hydrochloride Starting material medicine the most according to claim 1, it is characterized in that the capillary column (DB-624 that described capillary column uses 6 % cyanogen propyl group phenyl-94 % dimethyl polysiloxanes to be fixative, 0.53 mm × 30 m, 3.0 μm).
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| CN108614058A (en) * | 2018-06-19 | 2018-10-02 | 广西壮族自治区食品药品检验所 | Measure the headspace gas chromatography of glycine organic solvent residual in raw medicine amount |
| CN111812234A (en) * | 2020-06-30 | 2020-10-23 | 武汉九州钰民医药科技有限公司 | Method for detecting residual solvent in pantoprazole sodium sesquihydrate |
| CN112763603A (en) * | 2020-12-24 | 2021-05-07 | 四川欣美加生物医药有限公司 | Detection method of benzene content and application |
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