CN103185759A - Detection method for solvent residue in olanzapine and application for same - Google Patents
Detection method for solvent residue in olanzapine and application for same Download PDFInfo
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Abstract
The invention provides a detection method for solvent residue in olanzapine, which adopts a gas chromatographic method. The detection method provided by the invention is high in sensitivity and specificity, simple and fast to operate, and capable of rapidly and accurately detecting the organic solvents of acetonitrile, acetonitrile, acetone, triethylamine, methylbenzene, dimethylformamide (DMF) and dimethyl sulfoxide (DMSO) in olanzapine. The detection method can be used for quality control for olanzapine, lays the foundation for research, development and quality detection on the medicine, and has practical significance.
Description
Technical field
The invention belongs to the Pharmaceutical Analysis technical field, be specifically related to detection method and the application thereof of dissolvent residual in a kind of Olanzapine.
Background technology
(trade name: Zyprexa, English name: Olanzapine) chemistry 2-methyl-4-(4-methyl isophthalic acid-piperazinyl) by name-10H-thieno [2,3-b] [1,5] benzodiazepine, its structure is suc as formula shown in the I for Olanzapine.
Formula I
Olanzapine formulations is the product that Lilly Co., Eli. releases, and is a kind of antipsychotic drug, and multiple receptor system is had pharmacological action.Residual organic solvent acetonitrile, ethanol, acetone, triethylamine, toluene, dimethyl formamide (DMF), dimethyl sulfoxide (DMSO) (DMSO) can influence the security of medicine in the Olanzapine, therefore, need detect the acetonitrile in Olanzapine and the preparation thereof, ethanol, acetone, triethylamine, toluene, dimethyl formamide (DMF), dimethyl sulfoxide (DMSO) (DMSO).It is residual and meet the method for the drug standards need to set up to detect related solvents in Olanzapine and the related preparations thereof.
Summary of the invention
The purpose of this invention is to provide detection method and the application thereof of dissolvent residual in a kind of Olanzapine.This detection method adopts vapor-phase chromatography, and its chromatographic condition is as follows:
Chromatographic column: the capillary column of 6%-cyanogen propylbenzene-94%-dimethylsiloxane copolymer;
Carrier gas: be nitrogen, hydrogen, helium;
Flow rate of mobile phase: 0.2-5.0mL/min;
Detecting device: be FID, ECD, TCD;
Column temperature: 50～250 ℃.
Wherein:
The sample injection method of detection method can detect residual solvent in conjunction with the direct injected method for headspace injection method, also can detect residual solvent respectively for the direct injected method.
Carrier gas is preferably nitrogen.
Preferably, the solvent of dissolving test sample is dimethyl sulfoxide (DMSO) (DMSO), dimethyl formamide (DMF), methyl alcohol, water, is preferably dimethyl sulfoxide (DMSO) (DMSO), dimethyl formamide (DMF).
The concentration of need testing solution is 30-100mg/mL, is preferably 100mg/mL.
The sample size of direct injected method is 0.1-100 μ L, is preferably 1 μ L.
According to detection method provided by the invention, wherein, described chromatographic column is selected from DB-624 capillary column (30.0m * 0.53mm * 3.00 μ m), DM-624 capillary column (75.0m * 0.53mm * 3.00 μ m), DB-17 capillary column (30.0m * 0.53mm * 3.00 μ m), DB-35 capillary column (30.0m * 0.53mm * 3.00 μ m), HP-1 capillary column (30.0m * 0.53mm * 3.00 μ m), HP-5 capillary column (30.0m * 0.53mm * 3.00 μ m), DB-624 capillary column (30.0m * 0.53mm * 3.00 μ m) more preferably, DB-624 capillary column (60.0m * 0.53mm * 3.00 μ m) most preferably is DM-624 capillary column (75.0m * 0.53mm * 3.00 μ m).
According to detection method provided by the invention, wherein, the column temperature system of selection of described chromatographic column is constant temperature method and temperature programme, is preferably temperature programme.
According to detection method provided by the invention, wherein, the column temperature of headspace injection method is 50～250 ℃, preferred 50～120 ℃, and more preferably 50 ℃.
According to detection method provided by the invention, wherein, the column temperature of direct injected method is 50～250 ℃, preferred 50～120 ℃, and more preferably 60 ℃, 120 ℃.
According to detection method provided by the invention, wherein, the flow velocity of the phase that flows is 0.2-5.0mL/min, is preferably 3.0mL/min, 3.5mL/min.
According to detection method provided by the invention, wherein, the split ratio of headspace sampling is 1: 1-100: 100, be preferably 10: 1.
According to detection method provided by the invention, wherein, the split ratio of direct injected is 100: 1-1: 100, be preferably 5: 1.
According to detection method provided by the invention, detecting device is preferably FID (flame ionization ditector).
The present invention also provides the application of above-mentioned detection method in olanzapine formulations detects, and wherein, described olanzapine formulations is the form of tablet, capsule, granule, injection, controlled release preparation or sustained release preparation.
The detection method of dissolvent residual adopts vapor-phase chromatography to realize the rapid and accurate determination of the dissolvent residual in the Olanzapine in the Olanzapine provided by the invention, have higher sensitivity and specificity, simple to operation, degree of separation meets standard, and (that is, the degree of separation of residual solvent is all greater than 1.50.Degree of separation is the ratio of difference and average peak width of the retention time at adjacent two peaks, also is resolution, represents the separation degree at adjacent two peaks.R is more big, shows that the two adjacent groups separation is more good.When R＜1, two peaks overlap in general; When R=1.0, degree of separation can reach 98%; When R=1.5, degree of separation can reach 99.7%.Usually divide the sign that separates fully as two adjacent groups with R=1.5.When R=1, be called 4 σ and separate, two peaks separate substantially, and exposed peak area is 95.4%, inboard peak basic weight folded about 2%.During R=1.5, be called 6 σ and separate, exposed peak area is 99.7%.R 〉=1.5 are called fully and separate." Chinese pharmacopoeia regulation R should be greater than 1.5.Degree of separation computing formula: R=2 (tR2-tR1)/(W1+W2)), can be used for the quality control of Olanzapine, have realistic meaning.
Description of drawings
Fig. 1 is the gas chromatogram of standard solution among the embodiment 1;
Fig. 2 is the gas chromatogram of standard solution among the embodiment 3;
Fig. 3 is the gas chromatogram of standard solution among the embodiment 5.
Embodiment
Below in conjunction with embodiment the present invention is further described in detail, the embodiment that provides is only in order to illustrate the present invention, rather than in order to limit the scope of the invention.
Embodiment 1
1) instrument and testing conditions
The Agilent 7890N gas chromatograph that U.S. Agilent company produces, the G1888 head-space sampler, (the chromatographic column specification is the DM-624 capillary column of being produced by Di Ma company: 75.0m * 0.53mm * 3.00 μ m); Column temperature: kept 8 minutes for 50 ℃, be warming up to 200 ℃ with the heating rate of 20 ℃/min, kept 5 minutes; Vaporizer temperature: 250 ℃; Flow rate of carrier gas: nitrogen, 3.0mL/min; Detecting device: flame ionization ditector (FID); Detector temperature: 250 ℃; Head space heating-up temperature: 100 ℃; Equilibration time: 20 minutes; Sample size: 1mL, split ratio: 10: 1.
2) experimental procedure
Precision pipettes ethanol 158 μ L, acetonitrile 13 μ L, acetone 159 μ L, toluene 26 μ L, triethylamine 34 μ L, dimethyl formamide (DMF) 23 μ L in the 25mL measuring bottle that an amount of dimethyl sulfoxide (DMSO) (DMSO) is housed respectively, (DMSO) is diluted to scale with dimethyl sulfoxide (DMSO), mixing gets the standard stock solution; Precision is measured this liquid 1mL and is put in the 10mL measuring bottle, and (DMSO) is diluted to scale with dimethyl sulfoxide (DMSO), and mixing namely gets standard solution.Residual limit sees Table 1.
Table 1 dissolvent residual limit
Embodiment 2
1) instrument and testing conditions
The Agilent 7890N gas chromatograph that U.S. Agilent company produces, the G1888 head-space sampler, (the chromatographic column specification is the DM-624 capillary column of being produced by Di Ma company: 75.0m * 0.53mm * 3.00 μ m); Column temperature: kept 8 minutes for 50 ℃, be warming up to 200 ℃ with the heating rate of 20 ℃/min, kept 5 minutes; Vaporizer temperature: 250 ℃; Flow rate of carrier gas: nitrogen, 3.0mL/min; Detecting device: flame ionization ditector (FID); Detector temperature: 250 ℃; Head space heating-up temperature: 100 ℃; Equilibration time: 20 minutes; Sample size: 1mL, split ratio: 10: 1.
2) experimental procedure
Use the standard solution sample introduction among the embodiment 1.
Standard solution measurement result and precision test (n=6) are got standard solution 2mL and are put in the 10mL head space bottle, seal.Continuous sample introduction is measured successively, calculates the RSD% of acetonitrile, ethanol, acetone, triethylamine, toluene, dimethyl formamide peak area.Test findings sees Table 2.
Table 2 standard solution measurement result and precision test
The linear relationship test
Pipette standard stock solution 0.4,0.8,1.0,1.2 respectively, 1.8mL puts in the 25mL measuring bottle, (DMSO) is diluted to scale with dimethyl sulfoxide (DMSO), mixing is made into the test solution of variable concentrations; Get each solution 2mL respectively and put in the 10mL head space bottle, seal, sample introduction is measured successively.The result shows: acetonitrile is in the 0.01629-0.07330mg/mL concentration range, and linear relationship is good; Ethanol is in the 0.19971-0.89870mg/mL concentration range, and linear relationship is good; Acetone is in the 0.20047-0.90211mg/mL concentration range, and linear relationship is good; Triethylamine is in the 0.03971-0.17870mg/mL concentration range, and linear relationship is good; Toluene is in the 0.03598-0.16193mg/mL concentration range, and linear relationship is good.Dimethyl formamide (DMF) is in the 0.03489-0.15699mg/mL concentration range, and linear relationship is good.Test findings sees Table 3.
Table 3 linear relationship test findings
The standard solution stability test
Get standard solution 2mL respectively at 0h, 2h, 6h, 8h, 24h and put in the 10mL head space bottle, seal, headspace sampling is measured, the record chromatogram.Calculate the RSD% of the peak area of each solvent, see Table 4.The RSD% of acetonitrile, ethanol, acetone, triethylamine, toluene, dimethyl formamide (DMF) chromatographic peak integral area is respectively 5.35%, 2.53%, 0.35%, 0.13%, 0.51%, 4.76%, shows that acetonitrile, ethanol, acetone, triethylamine, toluene, dimethyl formamide (DMF) standard solution are basicly stable in 24h.
Table 4 standard solution stability test result (n=5)
1) instrument and testing conditions
The Agilent 7890N gas chromatograph that U.S. Agilent company produces, automatic sampler, (the chromatographic column specification is the DM-624 capillary column of being produced by Di Ma company: 75.0m * 0.53mm * 3.00 μ m); Column temperature: kept 7 minutes for 60 ℃, be warming up to 200 ℃ with the heating rate of 20 ℃/min, kept 9 minutes; Vaporizer temperature: 250 ℃; Flow rate of carrier gas: nitrogen, 3.5mL/min; Detecting device: flame ionization ditector (FID); Detector temperature: 250 ℃; Sample size: 1 μ L; Split ratio: 5: 1.
2) experimental procedure
Use the standard solution sample introduction among the embodiment 1.
Embodiment 4
1) instrument and testing conditions
The Agilent 7890N gas chromatograph that U.S. Agilent company produces, automatic sampler, (the chromatographic column specification is the DM-624 capillary column of being produced by Di Ma company: 75.0m * 0.53mm * 3.00 μ m); Column temperature: kept 7 minutes for 60 ℃, be warming up to 200 ℃ with the heating rate of 20 ℃/min, kept 9 minutes; Vaporizer temperature: 250 ℃; Flow rate of carrier gas: nitrogen, 3.5mL/min; Detecting device: flame ionization ditector (FID); Detector temperature: 250 ℃; Sample size: 1 μ L; Split ratio: 5: 1.
2) experimental procedure
Use the standard solution sample introduction among the embodiment 1.
Standard solution measurement result and precision test (n=6) are got standard solution 2mL and are put in the 10mL head space bottle, seal.Continuous sample introduction is measured successively, calculates the RSD% of acetonitrile, ethanol, acetone, triethylamine, toluene, dimethyl formamide (DMF) peak area.Test findings sees Table 5.
Table 5 standard solution measurement result and precision test
The linear relationship test
Pipette standard stock solution 0.4,0.8,1.0,1.2 respectively, 1.8mL puts in the 25mL measuring bottle, (DMSO) is diluted to scale with dimethyl sulfoxide (DMSO), mixing is made into the test solution of variable concentrations; Get each solution 2mL respectively and put in the 10mL head space bottle, seal, sample introduction is measured successively.The result shows: acetonitrile is in the 0.01629-0.07330mg/mL concentration range, and linear relationship is good; Ethanol is in the 0.19971-0.89870mg/mL concentration range, and linear relationship is good; Acetone is in the 0.20047-0.90211mg/mL concentration range, and linear relationship is good; Triethylamine is in the 0.03971-0.17870mg/mL concentration range, and linear relationship is good; Toluene is in the 0.03598-0.16193mg/mL concentration range, and linear relationship is good.Dimethyl formamide (DMF) is in the 0.03489-0.15699mg/mL concentration range, and linear relationship is good.Test findings sees Table 6.
Table 6 linear relationship test findings
The standard solution stability test
Get standard solution 2mL respectively at 0h, 2h, 6h, 8h, 24h and put in the 10mL head space bottle, seal, headspace sampling is measured, the record chromatogram.Calculate the RSD% of the peak area of each solvent, see Table 7.The RSD% of acetonitrile, ethanol, acetone, triethylamine, toluene, dimethyl formamide (DMF) chromatographic peak integral area is respectively 7.08%, 0.78%, 0.54%, 1.33%, 0.84%, 2.60%, shows that acetonitrile, ethanol, acetone, triethylamine, toluene, dimethyl formamide (DMF) standard solution are basicly stable in 24h.
Table 7 standard solution stability test result (n=5)
1) instrument and testing conditions
The Agilent 7890N gas chromatograph that U.S. Agilent company produces, automatic sampler, (the chromatographic column specification is the DM-624 capillary column of being produced by Di Ma company: 75.0m * 0.53mm * 3.00 μ m); Column temperature: kept 30 minutes for 120 ℃; Vaporizer temperature: 250 ℃; Flow rate of carrier gas: nitrogen, 3.5mL/min; Detecting device: flame ionization ditector (FID); Detector temperature: 250 ℃; Sample size: 1 μ L; Split ratio: 10: 1.
2) experimental procedure
Precision pipettes dimethyl sulfoxide (DMSO) (DMSO) 57 μ L in the 25mL measuring bottle that an amount of dimethyl formamide (DMF) is housed, and (DMF) is diluted to scale with dimethyl formamide, and mixing namely gets the standard stock solution; Precision is measured this liquid 1mL and is put in the 10mL measuring bottle, and (DMF) is diluted to scale with dimethyl formamide, and mixing namely gets standard solution.Residual limit sees Table 8.
Table 8 dissolvent residual limit
| Residual solvent | Proportion (g/mL) | Concentration (mg/mL) | Residual limit (%) |
| Dimethyl sulfoxide (DMSO) | 1.100 | 0.2508 | 0.5 |
| (DMSO) |
Embodiment 6
1) instrument and testing conditions
The Agilent 7890N gas chromatograph that U.S. Agilent company produces, automatic sampler, (the chromatographic column specification is the DM-624 capillary column of being produced by Di Ma company: 75.0m * 0.53mm * 3.00 μ m); Column temperature: kept 30 minutes for 120 ℃; Vaporizer temperature: 250 ℃; Flow rate of carrier gas: nitrogen, 3.5mL/min; Detecting device: flame ionization ditector (FID); Detector temperature: 250 ℃; Sample size: 1 μ L; Split ratio: 10: 1.
2) experimental procedure
Use the standard solution sample introduction among the embodiment 5.
Standard solution measurement result and precision test (n=6) are got standard solution 2mL and are put in the 10mL head space bottle, seal.Continuous sample introduction is measured successively, calculates the RSD% of dimethyl sulfoxide (DMSO) (DMSO) peak area.Test findings sees Table 9.
Table 9 standard solution measurement result and precision test
The linear relationship test
Pipette standard stock solution 0.4,0.8,1.0,1.2 respectively, 1.8mL puts in the 25mL measuring bottle, (DMF) is diluted to scale with dimethyl formamide, mixing is made into the test solution of variable concentrations; Get each solution 2mL respectively and put in the 10mL head space bottle, seal, sample introduction is measured successively.The result shows: dimethyl sulfoxide (DMSO) (DMSO) is in the 0.1003-0.4514mg/mL concentration range, and linear relationship is good.Test findings sees Table 10.
Table 10 linear relationship test findings
The standard solution stability test
Get standard solution 2mL respectively at 0h, 2h, 6h, 8h, 24h and put in the 10mL head space bottle, seal, headspace sampling is measured, the record chromatogram.Calculate the RSD% of the peak area of dimethyl sulfoxide (DMSO) (DMSO), see Table 11.The RSD% of the peak area of dimethyl sulfoxide (DMSO) (DMSO) is 1.96%, shows that dimethyl sulfoxide (DMSO) (DMSO) standard solution is basicly stable in 24h.
Table 11 standard solution stability test result (n=5)
Claims (9)
1. the detection method of an Olanzapine dissolvent residual is characterized in that, this detection method adopts vapor-phase chromatography, and its chromatographic condition is as follows:
Chromatographic column: the capillary column of 6%-cyanogen propylbenzene-94%-dimethylsiloxane copolymer;
Carrier gas: be nitrogen, hydrogen, helium;
Flow rate of mobile phase: 0.2-5.0mL/min;
Detecting device: be FID, ECD, TCD;
Column temperature: 50～250 ℃.
2. the detection method of a kind of Olanzapine dissolvent residual according to claim 1 is characterized in that, this detection method adopts vapor-phase chromatography, and its chromatographic condition is as follows:
Chromatographic column: the capillary column of 6%-cyanogen propylbenzene-94%-dimethylsiloxane copolymer;
Carrier gas: be nitrogen;
Flow rate of mobile phase: be 3.0mL/min or 3.5mL/min;
Detecting device: be FID (flame ionization ditector);
Column temperature: 50～120 ℃.
3. the detection method of a kind of Olanzapine dissolvent residual according to claim 2 is characterized in that, this detection method adopts vapor-phase chromatography, and its chromatographic condition is as follows:
Chromatographic column: the capillary column of 6%-cyanogen propylbenzene-94%-dimethylsiloxane copolymer;
Carrier gas: be nitrogen;
Flow rate of mobile phase: be 3.0mL/min or 3.5mL/min;
Detecting device: be FID (flame ionization ditector);
Column temperature: be 50 ℃, 60 ℃ or 120 ℃.
4. according to each described detection method of claim 1-3, described chromatographic column is selected from DB-624 capillary column (30.0m * 0.53mm * 3.00 μ m), DM-624 capillary column (75.0m * 0.53mm * 3.00 μ m), DB-17 capillary column (30.0m * 0.53mm * 3.00 μ m), DB-35 capillary column (30.0m * 0.53mm * 3.00 μ m), HP-1 capillary column (30.0m * 0.53mm * 3.00 μ m), HP-5 capillary column (30.0m * 0.53mm * 3.00 μ m); Be preferably DB-624 capillary column (30.0m * 0.53mm * 3.00 μ m), DB-624 capillary column (60.0m * 0.53mm * 3.00 μ m); DM-624 capillary column (75.0m * 0.53mm * 3.00 μ m) more preferably.
5. according to each described detection method of claim 1-3, the solvent of dissolving test sample is dimethyl sulfoxide (DMSO), dimethyl formamide, methyl alcohol, water, is preferably dimethyl sulfoxide (DMSO), dimethyl formamide.
6. according to each described detection method of claim 1-3, the concentration of need testing solution is 30-100mg/mL, is preferably 100mg/mL.
7. according to each described detection method of claim 1-3, the column temperature system of selection of described chromatographic column is constant temperature method or temperature programme, is preferably temperature programme.
8. each described detection method application in the detection of olanzapine formulations dissolvent residual of claim 1-3.
9. application according to claim 8, described olanzapine formulations are tablet, capsule, granule, injection, controlled release preparation or sustained release preparation.
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