CN108445110A - The detection method of residual solvent in a kind of semi-synthetic fish oil bulk pharmaceutical chemicals - Google Patents
The detection method of residual solvent in a kind of semi-synthetic fish oil bulk pharmaceutical chemicals Download PDFInfo
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Abstract
The invention discloses a kind of detection methods of residual solvent in semi-synthetic fish oil bulk pharmaceutical chemicals, A, take out sample from semi-synthetic fish oil bulk pharmaceutical chemicals, and aqueous isopropanol is added in semi-synthetic fish oil bulk pharmaceutical chemicals sample and is uniformly mixed so as to obtain isopropyl alcohol mixture；B, isopropyl alcohol mixture 2ml is taken, it is closed in top set empty bottle, ml headspace bottle is heated, the isopropyl alcohol mixture of ml headspace bottle is made to reach vapor liquid equilibrium；C, it takes in step B ml headspace bottle internal upper part gas to be injected into gas chromatograph and carries out separation determination；D, generated chromatogram in gas chromatograph is recorded, the residual solvent amount in semi-synthetic fish oil bulk pharmaceutical chemicals sample is obtained with calculated by peak area according to external standard method.The present invention has many advantages, such as that accuracy is high, specificity is strong, high sensitivity, reproducibility are good, can be qualitative or can quantitatively detect out residual solvent n-hexane in semi-synthetic fish oil, to ensure that the quality of semi-synthetic fish oil, improve the safety of clinical application.
Description
Technical field
The present invention relates to semi-synthetic fish oil raw material residual solvent detection method more particularly to a kind of semi-synthetic fish oil bulk pharmaceutical chemicals
The detection method of middle residual solvent.
Background technology
Semi-synthetic fish oil bulk pharmaceutical chemicals are a kind of fish oil bulk pharmaceutical chemicals, and semi-synthetic fish oil bulk pharmaceutical chemicals can remain molten in process of production
Agent, residual solvent are mainly n-hexane, need to detect the residual solvent levels contained in semi-synthetic fish oil bulk pharmaceutical chemicals, Ke Yizhi
Measure the quality of semi-synthetic fish oil bulk pharmaceutical chemicals with seeing.In the prior art, for the measurement hand of semi-synthetic fish oil bulk pharmaceutical chemicals quality
Section is complex, and sensitivity is not also high.
Invention content
Place in view of the shortcomings of the prior art, the purpose of the present invention is to provide in a kind of semi-synthetic fish oil bulk pharmaceutical chemicals
The detection method of residual solvent, can be qualitative or can quantitatively detect out residual solvent n-hexane in semi-synthetic fish oil, to ensure
The quality of semi-synthetic fish oil, the safety for improving clinical application.
The purpose of the invention is achieved by the following technical solution：
The detection method of residual solvent, method and step are as follows in a kind of semi-synthetic fish oil bulk pharmaceutical chemicals：
A, sample is taken out from semi-synthetic fish oil bulk pharmaceutical chemicals, aqueous isopropanol is added simultaneously in semi-synthetic fish oil bulk pharmaceutical chemicals sample
It is uniformly mixed so as to obtain isopropyl alcohol mixture, the proportioning between semi-synthetic fish oil bulk pharmaceutical chemicals sample and aqueous isopropanol is as follows：Every gram half
Synthesize the aqueous isopropanol that fish oil bulk pharmaceutical chemicals sample is added 1.3~1.4 milliliters；
B, the prepared isopropyl alcohol mixture 2ml of step A are taken, it is closed in top set empty bottle, ml headspace bottle is heated, is added
Hot temperature is 70 DEG C, 10 minutes heating times, the isopropyl alcohol mixture of ml headspace bottle is made to reach vapor liquid equilibrium；
C, it takes the ml headspace bottle internal upper part gas in step B to be injected into gas chromatograph and carries out separation determination, wherein chromatography
Condition is as follows：
Chromatographic column is HP-INNowax-60m × 0.32mm × 0.5 μm capillary column；
Carrier gas is nitrogen；
Detector in gas chromatograph uses fid detector, and the detector temperature of fid detector is 220 DEG C, gas phase color
The injector temperature of spectrometer is 200 DEG C, column flow 2mL/min, split ratio 20：1, ml headspace bottle internal upper part gas into
Sample amount is 1mL；The column oven of gas chromatograph constant temperature under 40 DEG C of temperature conditions is kept for 25 minutes；
D, generated chromatogram in gas chromatograph is recorded, semi-synthetic fish oil is obtained with calculated by peak area according to external standard method
Residual solvent amount in bulk pharmaceutical chemicals sample.
The present invention compared with the prior art, has the following advantages and advantageous effect：
The present invention has many advantages, such as that accuracy is high, specificity is strong, high sensitivity, reproducibility are good, can be qualitative or can quantify
Ground detects residual solvent n-hexane in semi-synthetic fish oil, to ensure that the quality of semi-synthetic fish oil, improve clinical application
Safety.
Description of the drawings
Fig. 1 is linear equation schematic diagram in table 3.2.P.5.3.
Specific implementation mode
The present invention is described in further detail with reference to embodiment：
Embodiment one
The detection method of residual solvent, method and step are as follows in a kind of semi-synthetic fish oil bulk pharmaceutical chemicals：
A, sample is taken out from semi-synthetic fish oil bulk pharmaceutical chemicals, aqueous isopropanol is added simultaneously in semi-synthetic fish oil bulk pharmaceutical chemicals sample
It is uniformly mixed so as to obtain isopropyl alcohol mixture, the proportioning between semi-synthetic fish oil bulk pharmaceutical chemicals sample and aqueous isopropanol is as follows：Every gram half
Synthesize the aqueous isopropanol that fish oil bulk pharmaceutical chemicals sample is added 1.3~1.4 milliliters；
Main component is omega-fatty acid triglycerides, semi-synthetic fish oil raw material in the semi-synthetic fish oil bulk pharmaceutical chemicals of the present invention
Medicine derives from standing grain major company of Britain (Croda International Plc), and n-hexane is used involved in the material synthesis processes
It is refined and is purified, the present invention needs to carry out residual solvent control to n-hexane.
It is semi-synthetic to be only embodied in this for the domestic detection method at present without residual solvent in disclosed semi-synthetic fish oil bulk pharmaceutical chemicals
In the import examination criteria of fish oil bulk pharmaceutical chemicals, the method which records needs to use HS-GC-MS as detection device, with sea
Foreign ethyl ester is detected as substrate, there is substrate to obtain difficult, experimental facilities requires the shortcomings of high.
The present invention selects, using HS-GC as detection device, using aqueous isopropanol as reaction dissolvent, with HP-INNowax to make
For chromatographic column, it is convenient to have many advantages, such as that experimental implementation is easy, experiment material obtains.
B, the prepared isopropyl alcohol mixture 2ml of step A are taken, it is closed in top set empty bottle, ml headspace bottle is heated, is added
Hot temperature is 70 DEG C, 10 minutes heating times, the isopropyl alcohol mixture of ml headspace bottle is made to reach vapor liquid equilibrium；
C, it takes in step B ml headspace bottle internal upper part gas to be injected into gas chromatograph and carries out separation determination, wherein chromatostrip
Part is as follows：
Chromatographic column is HP-INNowax-60m × 0.32mm × 0.5 μm capillary column；
Carrier gas is nitrogen；
Detector in gas chromatograph uses fid detector, and the detector temperature of fid detector is 220 DEG C, gas phase color
The injector temperature of spectrometer is 200 DEG C, column flow 2mL/min, split ratio 20：1, ml headspace bottle internal upper part gas into
Sample amount is 1mL；The column oven of gas chromatograph constant temperature under 40 DEG C of temperature conditions is kept for 25 minutes；
D, generated chromatogram in gas chromatograph is recorded, semi-synthetic fish oil is obtained with calculated by peak area according to external standard method
Residual solvent amount in bulk pharmaceutical chemicals sample.
Reference substance solution A experiments are as follows：
A, it takes n-hexane appropriate, adds isopropanol that the solution of the 2ug containing n-hexane in every milliliter of mixed solution is made, as a contrast
Product solution A；
B, the prepared reference substance solution A2ml of step A are taken, it is closed in top set empty bottle, ml headspace bottle is heated, is heated
Temperature is 70 DEG C, and 10 minutes heating times made the reference substance solution A of ml headspace bottle reach vapor liquid equilibrium；
C, it takes the ml headspace bottle internal upper part gas of reference substance solution A in step B to be injected into gas chromatograph and carries out separation survey
Fixed, wherein chromatographic condition is as follows：
Chromatographic column is HP-INNowax-60m × 0.32mm × 0.5 μm capillary column；
Carrier gas is nitrogen；
Detector in gas chromatograph uses fid detector, and the detector temperature of fid detector is 220 DEG C, gas phase color
The injector temperature of spectrometer is 200 DEG C, column flow 2mL/min, split ratio 20：1, ml headspace bottle internal upper part gas into
Sample amount is 1mL；The column oven of gas chromatograph constant temperature under 40 DEG C of temperature conditions is kept for 25 minutes；
D, generated chromatogram in gas chromatograph is recorded to be used as with reference to chromatogram A.
Reference substance solution B experiments are as follows：
A, take isopropanol that solution product solution B as a contrast is made；
B, the prepared reference substance solution B2ml of step A are taken, it is closed in top set empty bottle, ml headspace bottle is heated, is heated
Temperature is 70 DEG C, and 10 minutes heating times made the reference substance solution B of ml headspace bottle reach vapor liquid equilibrium；
C, it takes the ml headspace bottle internal upper part gas of reference substance solution B in step B to be injected into gas chromatograph and carries out separation survey
Fixed, wherein chromatographic condition is as follows：
Chromatographic column is HP-INNowax-60m × 0.32mm × 0.5 μm capillary column；
Carrier gas is nitrogen；
Detector in gas chromatograph uses fid detector, and the detector temperature of fid detector is 220 DEG C, gas phase color
The injector temperature of spectrometer is 200 DEG C, column flow 2mL/min, split ratio 20：1, ml headspace bottle internal upper part gas into
Sample amount is 1mL；The column oven of gas chromatograph constant temperature under 40 DEG C of temperature conditions is kept for 25 minutes；
D, generated chromatogram in gas chromatograph is recorded to be used as with reference to chromatogram B.
By generated chromatogram in above-mentioned test data sheet gas chromatograph, with reference to chromatogram A, with reference to chromatogram B, press
The residual solvent amount in semi-synthetic fish oil bulk pharmaceutical chemicals sample is obtained with calculated by peak area according to external standard method.
Embodiment two
The detection method of residual solvent, method and step are as follows in a kind of semi-synthetic fish oil bulk pharmaceutical chemicals：
A, 0.8 gram of sample is taken out from semi-synthetic fish oil bulk pharmaceutical chemicals, and 0.8 gram of semi-synthetic fish oil bulk pharmaceutical chemicals sample is added
1.1 milliliters of aqueous isopropanols are simultaneously uniformly mixed so as to obtain isopropyl alcohol mixture, as test solution；
B, the prepared isopropyl alcohol mixture 2ml of step A are taken, it is closed in top set empty bottle, ml headspace bottle is heated, is added
Hot temperature is 70 DEG C, 10 minutes heating times, the isopropyl alcohol mixture of ml headspace bottle is made to reach vapor liquid equilibrium；
C, it takes in step B ml headspace bottle internal upper part gas to be injected into gas chromatograph and carries out separation determination, wherein chromatostrip
Part is as follows：
Chromatographic column is HP-INNowax-60m × 0.32mm × 0.5 μm capillary column；
Carrier gas is nitrogen；
Detector in gas chromatograph uses fid detector, and the detector temperature of fid detector is 220 DEG C, gas phase color
The injector temperature of spectrometer is 200 DEG C, column flow 2mL/min, split ratio 20：1, ml headspace bottle internal upper part gas into
Sample amount is 1mL；The column oven of gas chromatograph constant temperature under 40 DEG C of temperature conditions is kept for 25 minutes；
D, generated chromatogram in gas chromatograph is recorded, semi-synthetic fish oil is obtained with calculated by peak area according to external standard method
Residual solvent amount in bulk pharmaceutical chemicals sample.
Embodiment three
The detection method of residual solvent, method and step are as follows in a kind of semi-synthetic fish oil bulk pharmaceutical chemicals：
A, sample 805.64mg is taken out from semi-synthetic fish oil bulk pharmaceutical chemicals, by the semi-synthetic fish oil bulk pharmaceutical chemicals samples of 805.64mg
1.1ml aqueous isopropanols are added and are uniformly mixed so as to obtain isopropyl alcohol mixture, as test solution；
Main component is omega-fatty acid triglycerides, semi-synthetic fish oil raw material in the semi-synthetic fish oil bulk pharmaceutical chemicals of the present invention
Medicine derives from standing grain major company of Britain (Croda International Plc), and n-hexane is used involved in the material synthesis processes
It is refined and is purified, the present invention needs to carry out residual solvent control to n-hexane.
B, the prepared isopropyl alcohol mixture 2ml of step A are taken, it is closed in top set empty bottle, ml headspace bottle is heated, is added
Hot temperature is 70 DEG C, 10 minutes heating times, the isopropyl alcohol mixture of ml headspace bottle is made to reach vapor liquid equilibrium；
C, it takes in step B ml headspace bottle internal upper part gas to be injected into gas chromatograph and carries out separation determination, wherein chromatostrip
Part is as follows：
Chromatographic column is HP-INNowax-60m × 0.32mm × 0.5 μm capillary column；
Carrier gas is nitrogen；
Detector in gas chromatograph uses fid detector, and the detector temperature of fid detector is 220 DEG C, gas phase color
The injector temperature of spectrometer is 200 DEG C, column flow 2mL/min, split ratio 20：1, ml headspace bottle internal upper part gas into
Sample amount is 1mL；The column oven of gas chromatograph constant temperature under 40 DEG C of temperature conditions is kept for 25 minutes；
D, generated chromatogram in gas chromatograph is recorded, semi-synthetic fish oil is obtained with calculated by peak area according to external standard method
Residual solvent amount in bulk pharmaceutical chemicals sample.
Reference substance solution A experiments are as follows：
A, n-hexane 10.24mg is taken, is placed in 50ml measuring bottles, adds isopropanol dissolving to be settled to scale, product store up as a contrast
Standby liquid；Precision measures reference substance storing solution 1ml, is placed in 100ml measuring bottles, adds isopropanol dissolving to be settled to scale, takes 2ml into top
In empty bottle, add isopropanol that the solution of the 2ug containing n-hexane in every milliliter of mixed solution is made, as a contrast product solution A；
B, the prepared reference substance solution A2ml of step A are taken, it is closed in top set empty bottle, ml headspace bottle is heated, is heated
Temperature is 70 DEG C, and 10 minutes heating times made the reference substance solution A of ml headspace bottle reach vapor liquid equilibrium；
C, it takes the ml headspace bottle internal upper part gas of reference substance solution A in step B to be injected into gas chromatograph and carries out separation survey
Fixed, wherein chromatographic condition is as follows：
Chromatographic column is HP-INNowax-60m × 0.32mm × 0.5 μm capillary column；
Carrier gas is nitrogen；
Detector in gas chromatograph uses fid detector, and the detector temperature of fid detector is 220 DEG C, gas phase color
The injector temperature of spectrometer is 200 DEG C, column flow 2mL/min, split ratio 20：1, ml headspace bottle internal upper part gas into
Sample amount is 1mL；The column oven of gas chromatograph constant temperature under 40 DEG C of temperature conditions is kept for 25 minutes；
D, generated chromatogram in gas chromatograph is recorded to be used as with reference to chromatogram A.
Reference substance solution B experiments are as follows：
A, take isopropanol that solution product solution B as a contrast is made；
B, the prepared reference substance solution B2ml of step A are taken, it is closed in top set empty bottle, ml headspace bottle is heated, is heated
Temperature is 70 DEG C, and 10 minutes heating times made the reference substance solution B of ml headspace bottle reach vapor liquid equilibrium；
C, it takes the ml headspace bottle internal upper part gas of reference substance solution B in step B to be injected into gas chromatograph and carries out separation survey
Fixed, wherein chromatographic condition is as follows：
Chromatographic column is HP-INNowax-60m × 0.32mm × 0.5 μm capillary column；
Carrier gas is nitrogen；
Detector in gas chromatograph uses fid detector, and the detector temperature of fid detector is 220 DEG C, gas phase color
The injector temperature of spectrometer is 200 DEG C, column flow 2mL/min, split ratio 20：1, ml headspace bottle internal upper part gas into
Sample amount is 1mL；The column oven of gas chromatograph constant temperature under 40 DEG C of temperature conditions is kept for 25 minutes；
D, generated chromatogram in gas chromatograph is recorded to be used as with reference to chromatogram B.
By generated chromatogram in above-mentioned test data sheet gas chromatograph, with reference to chromatogram A, with reference to chromatogram B, press
The residual solvent amount in semi-synthetic fish oil bulk pharmaceutical chemicals sample is obtained with calculated by peak area according to external standard method.
It takes in fish oil 807.64mg top set empty bottles, the 20 μ l of reference substance storing solution in reference substance solution A is added, add 1.1ml
Isopropanol is as mark-on test solution；It is analyzed by measuring method is drafted, sample is detection n-hexane under the chromatographic condition,
N-hexane reaches 2.08 with adjacent peak separating degree in mark-on sample, meets detection demand, method specificity is good.
Precision weighs n-hexane 10.24mg, sets in 50ml measuring bottles, adds isopropanol dissolving to be settled to scale, as a contrast product
Storing solution.Precision measures the reference substance stock solution, and according to the form below is diluted to the solution of various concentration step by step, by drafting method sample introduction 20
μ l record chromatogram, with log concentration value and peak area logarithm into line Regression.
It is method detection limit with 3~5 times of baseline noise, with 10 times or more the quantitative limits for method of baseline noise,
0.0512mg/ml (containing n-hexane 0.102ug in ml headspace bottle) (being equivalent to the 2.6% of limit concentration, signal-to-noise ratio 3.89) conduct
Detection limit, 0.1024mg/ml (containing n-hexane 0.205ug in ml headspace bottle) (are equivalent to the 5.1% of limit concentration, signal-to-noise ratio
12.72) it is used as quantitative limit, the range of linearity, sensitivity to be satisfied by residual solvent and measure requirement, statistical result is shown in Table
3.2.P.5.3 the range of linearity and table 3.2.P.5.3.5-4 quantitative limit repeatability.
The table 3.2.P.5.3.5-3 ranges of linearity
Table 3.2.P.5.3.5-4 quantitative limit repeatability
Accuracy test
Sample pipetting volume recovery test is carried out by the 50% of limit 5ug/ml, 100%, 150%.
Test sample：0001144924
Precision weighs n-hexane 10.24mg, sets in 50ml measuring bottles, adds isopropanol dissolving to be settled to scale, as a contrast product
Storing solution.Take test sample 15.61426g that storing solution 750ul is added in measuring bottle, mixing (contains n-hexane as mark-on sample
0.00984ug/mg), mark-on sample 0.2g (n=3), 0.4g (n=3), 0.6g (n=3) are weighed respectively, and sample-adding product make whole matter
Amount is about 0.8g, adds isopropanol 1.1ml, as test liquid 1#~9#, its content is surveyed according to established methodology, then compared with addition, counted
Calculate the rate of recovery.
Conclusion：By 50%~150% sample-adding recycling of limit concentration, the rate of recovery is put down between 86.85%~100.03%
It is 4.51% (n=9) that the equal rate of recovery, which is 92.22%, RSD, and method accuracy is good.It the results are shown in Table 3.2.P.5.3.5-6 haemolysis
Phosphatidyl choline and lysophosphatidyl ethanolamine accuracy test result.
Table 3.2.P.5.3.5-6 lysophosphatidyl cholines and lysophosphatidyl ethanolamine accuracy test result
Precision test
Test sample lot number：0001144924
Repeated experiment：Mark-on sample 0.4g (n=3) is weighed respectively, and sample-adding product make total quality be about 0.8g, add isopropyl
Alcohol 1.1ml, is measured totally by the method for drafting by 6 parts, calculates test sample concentration.
Intermediate precision is tested, and prepares 6 parts by repetitive test operation is parallel, in not same date, different analysis personnel survey
It is fixed.
Conclusion：The precision of method is good, the results are shown in Table 3.2.P.5.3.5-7 Precision test results.
Table 3.2.P.5.3.5-7 Precision test results
Solution stability testing
Test solution under repetitive test item is taken, is placed under room temperature, and was taken respectively at 0,2,4,5,13,24 hour
Sample measures.
Brief summary：This product is placed for 24 hours at room temperature, and n-hexane results change is little, and test solution is in interior for 24 hours steady under room temperature
It is fixed.It the results are shown in Table 3.2.P.5.3.5-8 solution stability testing results.
Table 3.2.P.5.3.5-8 solution stability testing results
Serviceability test
By test solution preparation method under repetitive test item, prepares, under basic chromatographic condition, prepare 11 parts respectively
Test solution finely tunes the amount that following chromatographic parameter measures n-hexane, calculates average value and RSD.
I injector temperature：195、205℃；
II detector temperature：215、225℃；
III column temperature：42℃；
Iv flow velocitys：2.2、1.8L/min.
V head space temperature：68℃.
Vi head space equilibration times：12、8min.
Conclusion：Above-mentioned condition slightly changes, and detection n-hexane repeatability is good, and separating degree is conformed to tailing factor
It asks, method good tolerance, the results are shown in Table 3.2.P.5.3.5-9 method serviceability test results.
Table 3.2.P.5.3.5-9 method serviceability test results
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement etc., should all be included in the protection scope of the present invention made by within refreshing and principle.
Claims (1)
1. the detection method of residual solvent in a kind of semi-synthetic fish oil bulk pharmaceutical chemicals, it is characterised in that：Its method and step is as follows：
A, sample is taken out from semi-synthetic fish oil bulk pharmaceutical chemicals, aqueous isopropanol and mixing is added in semi-synthetic fish oil bulk pharmaceutical chemicals sample
Isopropyl alcohol mixture is obtained, the proportioning between semi-synthetic fish oil bulk pharmaceutical chemicals sample and aqueous isopropanol is as follows：Every gram semi-synthetic
1.3~1.4 milliliters of aqueous isopropanol is added in fish oil bulk pharmaceutical chemicals sample；
B, the prepared isopropyl alcohol mixture 2ml of step A are taken, it is closed in top set empty bottle, ml headspace bottle is heated, heating temperature
Degree is 70 DEG C, 10 minutes heating times, the isopropyl alcohol mixture of ml headspace bottle is made to reach vapor liquid equilibrium；
C, it takes the ml headspace bottle internal upper part gas in step B to be injected into gas chromatograph and carries out separation determination, wherein chromatographic condition
It is as follows：
Chromatographic column is HP-INNowax-60m × 0.32mm × 0.5 μm capillary column；
Carrier gas is nitrogen；
Detector in gas chromatograph uses fid detector, and the detector temperature of fid detector is 220 DEG C, gas chromatograph
Injector temperature be 200 DEG C, column flow 2mL/min, split ratio 20：1, the sample size of ml headspace bottle internal upper part gas
For 1mL；The column oven of gas chromatograph constant temperature under 40 DEG C of temperature conditions is kept for 25 minutes；
D, generated chromatogram in gas chromatograph is recorded, semi-synthetic fish oil raw material is obtained with calculated by peak area according to external standard method
Residual solvent amount in medicine sample.
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Cited By (1)
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| CN113945647A (en) * | 2020-07-16 | 2022-01-18 | 鲁南制药集团股份有限公司 | Method for detecting ethanol and isopropanol in valsartan hydrochlorothiazide |
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