CN106940350A - A kind of method for determining multiple water-soluble vitamin in dimension belladonna solution again - Google Patents

A kind of method for determining multiple water-soluble vitamin in dimension belladonna solution again Download PDF

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Publication number
CN106940350A
CN106940350A CN201710114809.0A CN201710114809A CN106940350A CN 106940350 A CN106940350 A CN 106940350A CN 201710114809 A CN201710114809 A CN 201710114809A CN 106940350 A CN106940350 A CN 106940350A
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vitamin
solution
belladonna
dimension
reference substance
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薛泳
李�浩
韩洁
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Huaian No 1 Peoples Hospital
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Huaian No 1 Peoples Hospital
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
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  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Treatment Of Liquids With Adsorbents In General (AREA)

Abstract

The invention discloses a kind of method for determining multiple water-soluble vitamin in dimension belladonna solution again, this method is with vitamin B1, vitamin B2, vitamin B6For reference substance, precision draws reference substance solution and need testing solution, injects high performance liquid chromatograph, determines, and records collection of illustrative plates, produces the collection of illustrative plates of reference substance and test sample, obtained collection of illustrative plates is handled, to vitamin B in need testing solution1, vitamin B2, vitamin B6Carry out qualitative and quantify, and then calculate vitamin B in multiple dimension belladonna solution1, vitamin B2, vitamin B6Content.Each chromatographic peak separation of detection method is preferable, and baseline is steady, and peak type is good, and preferably, this method has good linear relationship, precision, stability, the rate of recovery to repeatability, can accurately detect vitamin B in multiple dimension belladonna solution1, vitamin B2, vitamin B6Component content, reach the purpose that quality control is carried out to multiple dimension belladonna solution.

Description

A kind of method for determining multiple water-soluble vitamin in dimension belladonna solution again
Technical field
The invention belongs to analysis technical field, and in particular to one kind determines multiple water-soluble vitamin in dimension belladonna solution again Method.
Background technology
Dimension belladonna solution is that the court Drug Manufacturing Room need fixed prescription system that is approved and preparing, use by oneself according to the court's clinic again Agent, is mainly used in spasmolysis and analgesia.It is usually used in treating gastrointestinal smooth muscle spasmic pain, and available for Nausea and vomiting, gastric acid secretion The treatment of excessive symptom, the also treatment available for indications such as courage renal colics.The preparation method of dimension belladonna solution is again:Take 50mL Belladonna tincture and 1mL Tween-80s are mixed, and then adding 316.3mL five with thread ties up in his oral administration solution, with adding with stirring, Finally add water and be settled to 1000ml, stir evenly and produce.It is equal that belladonna tincture, Tween-80 and five used by the party tie up his oral administration solution Bought for market, wherein primary raw material five ties up his oral administration solution and mainly includes vitamin B1, vitamin B2, vitamin B6Three kinds of dimensions Raw element, therefore, the content to vitamin in multiple dimension belladonna solution are controlled, and multivitamin separation detection are realized, to it Quality control has important practical significance.
The content of the invention
It is an object of the invention to provide a kind of method for determining multiple water-soluble vitamin in dimension belladonna solution again, to survey Tie up vitamin B in belladonna solution again calmly1, vitamin B2, vitamin B6Content, and then quality control is carried out to multiple dimension belladonna solution System.
The present invention is achieved by the following technical solutions:
A kind of method for determining multiple water-soluble vitamin in dimension belladonna solution again, comprises the following steps:
The preparation of reference substance solution:Weigh vitamin B1Reference substance, vitamin B2Reference substance, vitamin B6Reference substance, adds water molten Solution, is made every 1mL containing vitamin B16.0 μ g, vitamin B21.2 μ g, vitamin B61.8 μ g mixed reference substance solution;
The preparation of need testing solution:Multiple dimension belladonna solution is measured, add water constant volume, be made into every 1mL containing the μ L's of dimension belladonna solution 60 again Need testing solution;
Chromatographic condition is as follows:
Chromatographic column:5 μm of 4.6 × 250 mm of waters amino bondeds silica gel chromatographic column;
Mobile phase:Acetonitrile:30mmol/L potassium dihydrogen phosphate=80:20~75:25;
Flow velocity:0.9mL/min ~1.1mL/min;
Detection wavelength:278nm~282nm;
Column temperature:35℃~45℃;
Sample size:8μL ~12μL;
Theoretical cam curve:With vitamin B2Peak, which is calculated, is more than or equal to 2000;
Detection method:Precision draws reference substance solution and need testing solution, injects high performance liquid chromatograph, determines, and records collection of illustrative plates, The collection of illustrative plates of reference substance and test sample is produced, the detection data of establishing criteria product carry out linear regression, compare vitamin B1, vitamin B2, vitamin B6Equation of linear regression, to vitamin B in need testing solution1, vitamin B2, vitamin B6Carry out qualitative and quantify, And then calculate vitamin B in multiple dimension belladonna solution1, vitamin B2, vitamin B6Content.
The vitamin B1Equation of linear regression y=11633.27 x+13059.93, r=0.9996 are linear good.
The vitamin B2Equation of linear regression y=19021.23x+4234.75, r=0.9999 is linear good.
The vitamin B6Equation of linear regression y=11756.09 x+4430.02, r=0.9999 are linear good.
Further improvement project is the present invention:
The mobile phase is acetonitrile:30mmol/L potassium dihydrogen phosphate=75:25, column temperature is 40 DEG C, and Detection wavelength is 280 nm.
Further improvement project of the invention is:
The mobile phase is acetonitrile:30mmol/L potassium dihydrogen phosphate=80:20, column temperature is 45 DEG C, and Detection wavelength is 282 nm.
Further improvement project is the present invention:
The mobile phase is acetonitrile:30mmol/L potassium dihydrogen phosphate=75:25, column temperature is 35 DEG C, and Detection wavelength is 278 nm.
Beneficial effects of the present invention are:
Each chromatographic peak separation of detection method is preferable, and baseline is steady, and peak type is good, and preferably, this method has good repeatability Linear relationship, precision, stability, the rate of recovery, can accurately detect it is multiple dimension belladonna solution in vitamin B1, vitamin B2, dimension Raw element B6Component content, reach the purpose that quality control is carried out to multiple dimension belladonna solution.
Brief description of the drawings
Fig. 1 is the standard items spectrogram and test sample spectrogram of gained under the chromatographic condition of embodiment 1;
Fig. 2 is the standard items spectrogram and test sample spectrogram of gained under the chromatographic condition of embodiment 2;
Fig. 3 is the standard items spectrogram and test sample spectrogram of gained under the chromatographic condition of embodiment 3;
Fig. 4 is the gained chromatogram of embodiment 4;
Fig. 5 is vitamin B1The linear relationship chart of peak area value and concentration;
Fig. 6 is vitamin B2The linear relationship chart of peak area value and concentration;
Fig. 7 is vitamin B6The linear relationship chart of peak area value and concentration.
Embodiment
1st, instrument
Efficient liquid phase:The efficient liquid phase of Agilent 1260.
2nd, reagent:
Reference substance vitamin B1, vitamin B2, vitamin B6It is purchased from National Institute for Food and Drugs Control.
Belladonna is tieed up again:No.1 The People's Hospital, Huaian City makes by oneself.
Embodiment 1
The preparation of reference substance solution:Weigh vitamin B1Reference substance, vitamin B2Reference substance, vitamin B6Reference substance, adds water molten Solution, is made every 1mL containing vitamin B16.0 μ g, vitamin B21.2 μ g, vitamin B61.8 μ g mixed reference substance solution;
The preparation of need testing solution:The multiple dimension belladonna solution that lot number is 20160831 is measured, add water constant volume, be made into every 1mL containing multiple Tie up the μ L of belladonna solution 60 need testing solution;
Chromatographic condition is as follows:
Chromatographic column:5 μm of 4.6 × 250 mm of waters amino bondeds silica gel chromatographic column;
Mobile phase:Acetonitrile:30mmol/L potassium dihydrogen phosphate=75:25;
Flow velocity: 1mL/min;
Detection wavelength:280nm;
Column temperature:40℃;
Sample size:10μL;
Theoretical cam curve:With vitamin B2Peak, which is calculated, is more than or equal to 2000;
Detection method:Precision draws reference substance solution and need testing solution, injects liquid chromatograph, determines, and records collection of illustrative plates, such as schemes Shown in 1.
According to measurement result, vitamin B in belladonna solution is tieed up again1It should must not be less than 90 μ g/ml, vitamin B2It must not should lack In 35 μ g/ml, vitamin B,6It should must not be less than 30 μ g/ml.
Embodiment 2
The preparation be the same as Example 1 of reference substance solution and need testing solution.
Chromatographic condition is as follows:
Chromatographic column:5 μm of 4.6 × 250 mm of waters amino bondeds silica gel chromatographic column;
Mobile phase:Acetonitrile:30mmol/L potassium dihydrogen phosphate=80:20;
Flow velocity: 1mL/min;
Detection wavelength:282nm;
Column temperature:45℃;
Sample size:10μL;
Theoretical cam curve:With vitamin B2Peak, which is calculated, is more than or equal to 2000;
Detection method:Precision draws reference substance solution and need testing solution, injects liquid chromatograph, determines, and records collection of illustrative plates, such as schemes Shown in 2.
According to measurement result, vitamin B in belladonna solution is tieed up again1It should must not be less than 90 μ g/ml, vitamin B2It must not should lack In 35 μ g/ml, vitamin B,6It should must not be less than 30 μ g/ml.
Embodiment 3
The preparation be the same as Example 1 of reference substance solution and need testing solution.
Chromatographic condition is as follows:
Chromatographic column:5 μm of 4.6 × 250 mm of waters amino bondeds silica gel chromatographic column;
Mobile phase:Acetonitrile:30mmol/L potassium dihydrogen phosphate=75:25;
Flow velocity: 1mL/min;
Detection wavelength:278nm;
Column temperature:35℃;
Sample size:10μL;
Theoretical cam curve:With vitamin B2Peak, which is calculated, is more than or equal to 2000;
Detection method:Precision draws reference substance solution and need testing solution, injects liquid chromatograph, determines, and records collection of illustrative plates, such as schemes Shown in 3.
According to measurement result, vitamin B in belladonna solution is tieed up again1It should must not be less than 90 μ g/ml, vitamin B2It must not should lack In 35 μ g/ml, vitamin B,6It should must not be less than 30 μ g/ml.
Embodiment 4
Interference test
The preparation be the same as Example 1 of reference substance solution.
The preparation of full auxiliary material solution:Belladonna tincture and Tween-80 are measured, add water constant volume, be made into every 1mL μ containing belladonna tincture 3 L, the μ L of Tween-80 0.06 full auxiliary material solution;
Chromatographic condition be the same as Example 1.
Detection method:Precision draws reference substance solution, full auxiliary material solution and blank solvent(That is water), inject liquid chromatogram Instrument, is determined, and records collection of illustrative plates, as shown in Figure 4.
According to measurement result, auxiliary material with blank solvent in peak position without absworption peak, it is noiseless to assay.
Embodiment 5
Vitamin B1Equation of linear regression
By reference substance vitamin B11.21 μ g/ml, 2.42 μ g/ml, 3.63 μ g/ml, 4.84 μ g/ml, 6.06 μ g/ are configured to respectively Ml, 8.48 μ g/ml standard liquid, according to the chromatographic condition of embodiment 1, each precision measures 10 μ L injection liquid chromatographs, often Individual titer continuous sample introduction three times, records chromatogram, peak area is determined, with peak area value(S)To concentration(C)Linearly returned Return, try to achieve the equation of linear regression of vitamin B1:The x+13059.93 of y=11633.27 is simultaneously made with peak area value S to concentration C Figure, obtains a rectilinear, measurement result is shown in Table 1, Fig. 5.
The vitamin B1 linear determination data of table 1
Conclusion:Vitamin B1Equation of linear regression y=11633.27 x+13059.93, r=0.9996 is linearly good.
Embodiment 6
Vitamin B2Equation of linear regression
By reference substance vitamin B20.24 μ g/ml, 0.48 μ g/ml, 0.71 μ g/ml, 0.95 μ g/ml, 1.19 μ g/ are configured to respectively Ml, 1.66 μ g/ml standard liquid, according to the chromatographic condition of embodiment 1, each precision measures 10 μ L injection liquid chromatographs, often Individual titer continuous sample introduction three times, records chromatogram, peak area is determined, with peak area value(S)To concentration(C)Linearly returned Return, try to achieve the equation of linear regression of vitamin B2:The x+13059.93 of y=11633.27 is simultaneously made with peak area value S to concentration C Figure, obtains a rectilinear, measurement result is shown in Table 2, Fig. 6.
The vitamin B2 linear determination data of table 2
Conclusion:Vitamin B2Equation of linear regression y=19021.23x+4234.75, r=0.9999 are linearly good.
Embodiment 7
Vitamin B6Equation of linear regression
By reference substance vitamin B60.39 μ g/ml, 0.77 μ g/ml, 1.16 μ g/ml, 1.55 μ g/ml, 1.93 μ g/ are configured to respectively Ml, 2.71 μ g/ml standard liquid, according to the chromatographic condition of embodiment 1, each precision measures 10 μ L injection liquid chromatographs, often Individual titer continuous sample introduction three times, records chromatogram, peak area is determined, with peak area value(S)To concentration(C)Linearly returned Return, try to achieve vitamin B6Equation of linear regression:The x+4430.02 of y=11756.09, and concentration C is made with peak area value S Figure, obtains a rectilinear, measurement result is shown in Table 3, Fig. 7.
The vitamin B of table 36Linear determination data
Conclusion:Vitamin B6Equation of linear regression y=11756.09 x+4430.02, r=0.9999 is linearly good.
Embodiment 8
Sample introduction precision test
Reference substance solution preparation method and chromatographic condition be the same as Example 1, take reference substance solution, and continuous sample introduction 5 times records chromatogram Figure, measurement result is shown in Table 4.
The sample introduction Precision test result of table 4
Number of injections 1 2 3 4 5 It is average RSD%
Vitamin B1Peak area(S) 83299 82834 83062 82979 82687 82972 0.28
Vitamin B2Peak area(S) 25598 25434 25618 25549 25487 25537 0.30
Vitamin B6Peak area(S) 26600 26517 26619 26783 26487 26601 0.43
Conclusion:From table 4, result of the test vitamin B1RSD% is 0.28%(n=5), vitamin B2RSD% is 0.30%(n= 5), vitamin B6RSD% is 0.43%(n=5), show that sample introduction precision is preferable.
Embodiment 9
Recovery test
Vitamin B is taken respectively1, vitamin B2, vitamin B6Be made into standard liquid, each sample according to embodiment 1 chromatographic condition and Detection method is determined, and calculates the rate of recovery, and measurement result is shown in Table 5, table 6, table 7.
The vitamin B of table 51Recovery test result
The vitamin B of table 62Recovery test result
The vitamin B of table 76Recovery test result
Conclusion:By table 5, table 6, table 7 is visible, vitamin B1Average recovery rate is that 95.35%, RSD is 3.79%, vitamin B2It is average The rate of recovery is that 102.40%, RSD is 2.80%, vitamin B6Average recovery rate is that 94.66%, RSD is 2.76%, show the rate of recovery compared with It is good.
Embodiment 10
Replica test
6 parts of the sample that lot number is 160831 is taken, test sample is prepared according to the method for embodiment 1, according to the chromatostrip of embodiment 1 Part, each precision measures 10 μ L injection liquid chromatographs, records chromatogram, measurement result is shown in Table 8.
The repeated measurement result of table 8(n=6)
Solution sequence number Vitamin B2Content Vitamin B6Content Vitamin B1Content
Sample 1 0.0456 0.0412 0.1126
Sample 2 0.0463 0.0417 0.1096
Sample 3 0.0458 0.0416 0.1192
Sample 4 0.0460 0.0414 0.1184
Sample 5 0.0459 0.0413 0.1168
Average content 0.0459 0.0415 0.1138
RSD 0.76% 0.74% 4.30%
Conclusion:From table 8, result of the test vitamin B2RSD is 0.76%, vitamin B6RSD is 0.74%, vitamin B1 RSD shows repeated preferable for 4.30%.
Embodiment 11
Chromatographic condition durability change in flow
According to the experimental method of embodiment 1, flow velocity is changed into:0.9ml/min, 1.1ml/min are investigated between multivitamin Peak separating degree, the results are shown in Table 9
The change in flow test result table of table 9
Conclusion:Determined under this chromatographic condition, it is seen that change flow velocity in the range of 0.9ml/min ~ 1.1ml/min conditions permits Separating degree detection is had not significant impact.
Embodiment 12
Chromatographic condition durability sample size changes
According to the experimental method of embodiment 1, sample size is changed into:8 μ l, 12 μ l investigate the peak separating degree between multivitamin, It the results are shown in Table 10.
The sample size of table 10 changes test result table
Conclusion:Determined under this chromatographic condition, it is seen that flow velocity is changed in the range of the μ l conditions permits of 8 μ l ~ 12 separating degree is detected Have not significant impact.

Claims (4)

1. a kind of method for determining multiple water-soluble vitamin in dimension belladonna solution again, it is characterised in that comprise the following steps:
The preparation of reference substance solution:Weigh vitamin B1Reference substance, vitamin B2Reference substance, vitamin B6Reference substance, adds water molten Solution, is made every 1mL containing vitamin B16.0 μ g, vitamin B21.2 μ g, vitamin B61.8 μ g mixed reference substance solution;
The preparation of need testing solution:Multiple dimension belladonna solution is measured, add water constant volume, be made into every 1mL containing the μ L's of dimension belladonna solution 60 again Need testing solution;
Chromatographic condition is as follows:
Chromatographic column:5 μm of 4.6 × 250 mm of waters amino bondeds silica gel chromatographic column;
Mobile phase:Acetonitrile:30mmol/L potassium dihydrogen phosphate=80:20~75:25;
Flow velocity:0.9mL/min ~1.1mL/min;
Detection wavelength:278nm~282nm;
Column temperature:35℃~45℃;
Sample size:8μL ~12μL;
Theoretical cam curve:With vitamin B2Peak, which is calculated, is more than or equal to 2000;
Detection method:Precision draws reference substance solution and need testing solution, injects high performance liquid chromatograph, determines, and records collection of illustrative plates, The collection of illustrative plates of reference substance and test sample is produced, the detection data of establishing criteria product carry out linear regression, compare vitamin B1, vitamin B2, vitamin B6Equation of linear regression, to vitamin B in need testing solution1, vitamin B2, vitamin B6Carry out qualitative and quantify, And then calculate vitamin B in multiple dimension belladonna solution1, vitamin B2, vitamin B6Content.
2. a kind of method for determining multiple water-soluble vitamin in dimension belladonna solution again according to claim 1, its feature It is:The mobile phase is acetonitrile:30mmol/L potassium dihydrogen phosphate=75:25, column temperature is 40 DEG C, and Detection wavelength is 280 nm.
3. a kind of method for determining multiple water-soluble vitamin in dimension belladonna solution again according to claim 1, its feature It is:The mobile phase is acetonitrile:30mmol/L potassium dihydrogen phosphate=80:20, column temperature is 45 DEG C, and Detection wavelength is 282 nm.
4. a kind of method for determining multiple water-soluble vitamin in dimension belladonna solution again according to claim 1, its feature It is:The mobile phase is acetonitrile:30mmol/L potassium dihydrogen phosphate=75:25, column temperature is 35 DEG C, and Detection wavelength is 278 nm.
CN201710114809.0A 2017-02-28 2017-02-28 A kind of method for determining multiple water-soluble vitamin in dimension belladonna solution again Pending CN106940350A (en)

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Cited By (1)

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CN106908536A (en) * 2017-02-28 2017-06-30 淮安市第人民医院 A kind of method for determining multiple water-soluble vitamin in general celebrating solution

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