CN106442790A - Method for detection of B vitamins - Google Patents

Method for detection of B vitamins Download PDF

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Publication number
CN106442790A
CN106442790A CN201610882137.3A CN201610882137A CN106442790A CN 106442790 A CN106442790 A CN 106442790A CN 201610882137 A CN201610882137 A CN 201610882137A CN 106442790 A CN106442790 A CN 106442790A
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vitamin
phase
detection method
mobile phase
volume fraction
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苏昭仑
叶少文
游景水
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BY Health Co Ltd
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BY Health Co Ltd
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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
    • 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
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/06Preparation

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
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Abstract

The invention relates to the field of analytical chemistry, in particular to a method for the detection of B vitamins. Experiments show that the method can be used for detecting many kinds of vitamin sustained-release capsules, wherein the detection peak of each excipient does not interfere with the detection of the B vitamins. The method is good in accuracy, precision, stability and repeatability.

Description

A kind of detection method of vitamin B group
Technical field
The present invention relates to analytical chemistry field, more particularly, to a kind of detection method of vitamin B group.
Background technology
Vitamin is to safeguard health, enhancing development and a class organic compound necessary to regulation of physiological functions Thing.These compounds are all present in natural food, typically can not synthesize in vivo or synthetic quantity less it is impossible to meet needs. Due to dietary habit with lack nutrient knowledge, and modern's lifestyle change is it is difficult to reach preferable balanced diet pattern, According to authoritative department investigation, Chinese majority's diet can not equalize some vitamin of offer and mineral, calcium deficiency, ferrum, dimension life Plain A, B2 are commonplace, zinc deficiency, selenium, vitamin B1, vitamin C also very common.It is therefore desirable to taking nutrient prime replenisher.
Multivitamin slow releasing capsule is the effect reaching slow release by hydrogel matrix, meets Digestive system and occur after being administered orally Hydration generates gel, and vitamin B group therein is discharged by way of diffusion and gel skeleton corrosion.Hydrogel matrix It is not easy to be completely dissolved, thus causing vitamin B group assay difficulty big.Through test, report that the method for document is equal at present The vitamin B in multivitamin slow releasing capsule can not be measured1、B2、B3、B5、B6、B7、B12.
In links such as the production of health food, storage, supply and Clinical practice, for guaranteeing health food quality, all Through strict analytical control, the safely and effectively reasonable of health food need to be ensured with this.Therefore, multiple dimension lifes are developed further In plain slow releasing capsule, the detection method of vitamin B group is non-the normally off key.
Content of the invention
In view of this, the technical problem to be solved in the present invention is to provide a kind of detection method of vitamin B group, the present invention Using method associated with HPLC-MS, can achieve the detection to 7 kinds of vitamin B group in multivitamin slow releasing capsule, party's normal Property scope wide, precision, repeatability, stability and sensitivity, accuracy are all good, and blank solution is to measurement result no shadow Ring.
The detection method of the vitamin B group that the present invention provides, with aqueous formic acid or acetic acid aqueous solution for mobile phase A phase; With methanol or acetonitrile for Mobile phase B phase;Using High performance liquid chromatography mass spectrometry, sample is detected, according to mass spectrum and Chromatogram carries out qualitative and/or quantitative to vitamin B group;
Described high performance liquid chromatography adopts gradient elution, and elution program is:
0~0.5min, the volume fraction of mobile phase A phase is 92%;
0.5min~8min, the volume fraction of mobile phase A phase is down to 10% by 92%;
8min~8.5min, the volume fraction of mobile phase A phase is 10%;
8.5min~9min, the volume fraction of mobile phase A phase rises to 92% by 10%;
9min~12min, the volume fraction of mobile phase A phase is 92%.
HPLC is had selection to the separating power of complex sample with MS by High performance liquid chromatography mass spectrometry (HPLC-MS) Property, susceptiveness and combining a little of relative molecular mass and structural information can be provided, medicine, food, health product or The multiple fields such as environmental analyses are widely used.But when in the face of needing a kind of new sample is detected, need The condition of HPLC-MS is groped, to set up the detection method for this sample.New method needs to carry out precision, weight Renaturation and the many identifications of accuracy, show to the qualification result of the method provided by the present invention:
Linearly:Linear Experiment result shows, vitamin B1, the coefficient R of B2, B3, B5, B6, B7, B12 are respectively 0.9999th, 0.9998,0.9998,0.9998,0.9998,0.9998,0.9997, thus with the method measure vitamin B1, B2, B3, B5, B6, B7, B12 concentration is respectively 1.57343 μ g/ml to 7.86712 μ g/ml, 1.59031 μ g/ml to 7.95156 μ g/ Ml, 10.0300 μ g/ml to 50.1498 μ g/ml, 3.21878 μ g/ml to 16.0939 μ g/ml, 1.57642 μ g/ml are extremely 7.88211 μ g/ml, 0.524892 μ g/ml to 2.62446 μ g/ml, 0.534886 μ g/ml to 2.67443 μ g/ml, between present Good is linear, meets GB/T27404-2008《Good Laboratory controls specification》Requirement (GB/T27404-2008 require phase Close coefficients R >=0.99).
Precision:Same portion vitamin B group standard working solution, continuous sample introduction six times, 7 kinds of vitamin B group peak areas Relative standard deviation is smaller than 0.8%, illustrates that the precision of the method is good.
Repeatability:Take vitamin B group standard working solution, weigh 6 parts by same analysis personnel's precision, operation repetitive measures 6 parts of need testing solutions, result shows, 7 kinds of vitamin B group content relative standard deviations are smaller than 0.9%, in prescribed limit, The repeatability of this method provided by the present invention is described preferably.
Stability:The standard working solution of vitamin B group is placed after 0h, 1h, 2h, 4h, 8h, 12h respectively at room temperature Detected, the relative standard deviation of 7 kinds of vitamin B group peak areas is smaller than 0.7%, illustrated that the precision of the method is good.
Blank experiment shows, in the detection spectrogram of blank solution, in vitamin B1, the going out of B2, B3, B5, B6, B7, B12 Equal no peak at peak time, shows blank substantially noiseless to measurement result.
Accuracy:Add the standard substance of known quantity in the sample, with the method that the present invention provides, vitamin B group is carried out Quantitative, calculate average recovery.Every group of concentration detects the response rate parallel three times, calculates meansigma methodss, result shows, 7 kinds of B races dimension lifes The plain response rate is located at 99.1%~100.1%, meets the response rate and requires.Illustrate that the method has good accuracy.
Liquid chromatograph be sample component between column packing and mobile phase mass exchange and reach detached purpose, therefore will Flowing relative sample is asked to have certain solvability and do not produce chemical reaction with sample, its viscosity is as far as possible little, so that The separating effect having arrived;And the physico-chemical property of mobile phase will be adapted with the detector using.As used UV-detector, then should Prepared using the solvent relatively low to uv absorption.Its boiling point can not ether low, otherwise easily produce bubble, lead to experiment cannot enter OK.For vitamin B group, the mobile phase being provided with the present invention is carried out isocratic elution and ensure that more preferable Detection results, Testing result better than other mobile phases.
In the present invention, in aqueous formic acid, the volume fraction of formic acid is 0.1%;In described acetic acid aqueous solution, acetic acid Volume fraction is 0.1%.
In some specific embodiments, the aqueous formic acid that mobile phase A phase is 0.1% for volume fraction.
In further embodiments, the acetic acid aqueous solution that mobile phase A phase is 0.1% for volume fraction.
In the present invention, the flow velocity of mobile phase of high performance liquid chromatography is 0.3mL/min~0.5mL/min.
In some specific embodiments, the flow velocity of mobile phase of high performance liquid chromatography is 0.5mL/min.
Selection to column temperature need to consider the material to be separated characteristic of itself, and column temperature affects the dissolving to test substance for the mobile phase Degree also can affect post pressure.Generally, improve column temperature to be conducive to improving separating degree, but temperature is too high, and that post can be led to press through be low, It is unfavorable for the detection of material.
In the present invention, the column temperature of the chromatographic column of high performance liquid chromatography is 30 DEG C~40 DEG C.
In some specific embodiments, the column temperature of the chromatographic column of high performance liquid chromatography is 40 DEG C.
The sample size of high performance liquid chromatography is 1~5 μ L, preferably 2 μ L.
For the method that the present invention provides, the polarity according to vitamin B group selects C18 chromatographic column.The size of chromatographic column Impact can be produced on separating resulting, its internal diameter can produce impact, the shorter chromatographic column run time of length to the flow velocity of mobile phase Short, post pressure is relatively low;The longer chromatographic column resolution original text of length, but run time increases.
In the present invention, the chromatographic column of high performance liquid chromatography is C18 chromatographic column, a size of 100 × 4.6mm, 2.6 μm;150× 4.6mm, 2.7 μm or 100 × 4.6mm, 3 μm.
In some embodiments, chromatographic column is Phenomenex, Kinetex, XB-C18, (100 × 4.6mm, 2.6 μm); Agilent, EC-C18, (150 × 4.6mm, 2.7 μm);Or Phenomenex, Luna, C18 (2), (100 × 4.6mm, 3 μm).
In one specific embodiment, chromatographic column is Phenomenex, Kinetex, XB-C18, (100 × 4.6mm, 2.6 μ m).
In the present invention, mass spectrographic ion source is electron spray positive ion source;Ion source temperature is 600 DEG C.
In the present invention, mass spectrographic electron spray voltage is 5500V;Collision air pressure 7.0psi;Gas curtain air pressure 22.0psi;Atomization Air pressure 60.0psi;Secondary air speed 20.0psi.
Detection parameter such as table 1 to different vitamin B group:
Table 1 mass spectrometry parameters
Wherein, parent ion (Q1), quantitative and qualitative ion pair (Q3), go cluster voltage (DP), entrance potential (EP), collision cell to enter Mouth voltage (CEP), collision gas energy (CE), collision cell exit potential (CXP).
Same impact is notable on testing result for the pretreatment mode of sample, and improperly pre-treatment can lead to detect unsuccessfully.
Through pre-treatment before inventive samples sample introduction, the mode of described pre-treatment is:With water for solvent to the sample after pulverizing Carry out supersound extraction, filtration sterilization after centrifugation;The time of described supersound extraction is 20~40min;Temperature is 10~30 DEG C of work( Rate is 0.8~1.1KW, and frequency is 37~45KHz.
In pretreatment process, water is (90mg~180mg) with the quality-volume ratio of sample:(500mL~1000mL).
The ultrasonic time is 30min.
The rotating speed of centrifugation is 8000r/min;Time is 4~8min.Preferably it is centrifuged 5min.
Take supernatant liquid filtering degerming after centrifugation, filter footpath is 0.22 μm.
Application in the detection method that the present invention provides vitamin B group detection in health product.
The health product that the method provided by the present invention is suitable for are multivitamin slow releasing capsule.
In described multivitamin slow releasing capsule, adjuvant includes:Sodium alginate, polyvinyl alcohol, polyvinyl pyrrolidone.
Experiment shows, using the method that the present invention provides, multivitamin slow releasing capsule is detected, adjuvant therein The detection peak of composition will not to vitamin B group produce interference, the present invention provide method have good accuracy, precision, Stability and repeatability.
Brief description
Fig. 1~7 show the standard curve of vitamin B1, B2, B3, B5, B6, B7, B12 successively;
Fig. 8~14 show the chromatogram contrast of vitamin B1, the mark product of B2, B3, B5, B6, B7, B12 and pure water successively;Its Middle Fig. 8-a~Figure 14-a shows the chromatogram of the mark product of vitamin B1, B2, B3, B5, B6, B7, B12, and Fig. 8-b~Figure 14-b shows pure The chromatogram of water purification.
Specific embodiment
The invention provides a kind of detection method of vitamin B group, those skilled in the art can use for reference present disclosure, suitable When modified technique parameter is realized.Specifically, all similar replacements and change for a person skilled in the art It is it will be apparent that they are considered as including in the present invention.The method of the present invention and application are entered by preferred embodiment Go description, related personnel substantially can be carried out to methods herein and application in without departing from present invention, spirit and scope Change or suitably change and combine, to realize and to apply the technology of the present invention.
The instrument that the present invention adopts and reagent are all common commercially available product, all can buy in market.
Wherein:
Instrument is Agilent 1260 high performance liquid chromatograph-API3200 mass spectrograph (joining ESI ion source).
Reagent reagent:Formic acid (chromatographically pure);Methanol (chromatographically pure);One-level water;Vitamin B1-thiamine nitrate (source: SUPELCO, lot number:LB84083V, purity:99.9%);Vitamin B2-riboflavin (source:Dr., lot number:31106, purity: 98.9%);Vitamin B3-nicotiamide (source:SUPELCO, lot number:LC01839V, purity:99.9%);Vitamin B5-pantothenic acid Calcium (source:SUPELCO, lot number:LC11592V, purity:99.9%);Vitamin B6-pyridoxine hydrochloride (source:SUPELCO, Lot number:LB83988V, purity:99.9%);Vitamin B7-biotin (source:National Institute for Food and Drugs Control, lot number: 100291-201303, purity:99.6%);Vitamin B12-cobalamine (source:National Institute for Food and Drugs Control, lot number: 100248-201203, purity:90.2%).
With reference to embodiment, the present invention is expanded on further:
Embodiment 1
High performance liquid chromatograph condition:
Mobile phase:A:0.1% formic acid solution, B:Methanol, gradient elution;
Flow velocity:0.5ml/min;
Column temperature:40℃;
Chromatographic column:Phenomenex, Kinetex, XB-C18,100 × 4.6mm, 2.6 μm.
Mass spectrometry parameters such as table 1:
Table 1 mass spectrometry parameters
Ion source temperature is 600 DEG C, and mass spectrographic electron spray voltage is 5500V;Collision air pressure 7.0psi;Gas curtain air pressure 22.0psi;Atomization air pressure 60.0psi;Secondary air speed 20.0psi.
Precision weighs thiamine nitrate 5.25mg, riboflavin 5.36mg, nicotiamide 5.02mg, calcium pantothenate 5.37mg respectively, Pyridoxine hydrochloride 5.26mg, biotin 5.27mg, cobalamine 5.93mg, are respectively placed in 50ml brown volumetric flask, add water-soluble Solve and be settled to scale, shake up, obtain final product storing solution.Storing solution is placed in 4 DEG C of refrigerator and stores for future use.(note:Riboflavin need to first add After a small amount of hydrochloric acid solution dissolving, add water constant volume.)
Accurate absorption thiamine nitrate storing solution 3.00ml respectively, riboflavin storing solution 3.00ml, nicotiamide storing solution 20.00ml, calcium pantothenate storing solution 6.00ml, pyridoxine hydrochloride storing solution 3.00ml, biotin storing solution 1.00ml, cobalamine stores up Standby liquid 1.00ml, is placed in 100ml brown volumetric flask, adds water to be settled to scale, shakes up, and obtains final product working solution, accurate respectively Draw working solution 1 μ l, 2 μ l, 3 μ l, 4 μ l, 5 μ l, be analyzed measuring, draw standard working curve.Result such as table 2:
Table 2:Test data
Linear evaluation:Vitamin B1, B2, B3, B5, B6, B7, B12 coefficient R be respectively 0.9999,0.9998, 0.9998th, 0.9998,0.9998,0.9998,0.9997, thus with the method measure vitamin B1, B2, B3, B5, B6, B7, B12 concentration is respectively 1.57343 μ g/ml to 7.86712 μ g/ml, 1.59031 μ g/ml to 7.95156 μ g/ml, 10.0300 μ g/ Ml to 50.1498 μ g/ml, 3.21878 μ g/ml to 16.0939 μ g/ml, 1.57642 μ g/ml to 7.88211 μ g/ml, 0.524892 μ g/ml to 2.62446 μ g/ml, 0.534886 μ g/ml to 2.67443 μ g/ml, between assume good linear, symbol Close GB/T27404-2008《Good Laboratory controls specification》Requirement【GB/T27404-2008 requirement coefficient R >= 0.99】.
Embodiment 2
Accurate absorption thiamine nitrate storing solution 3.00ml respectively, riboflavin storing solution 3.00ml, nicotiamide storing solution 20.00ml, calcium pantothenate storing solution 6.00ml, pyridoxine hydrochloride storing solution 3.00ml, biotin storing solution 1.00ml, cobalamine stores up Standby liquid 1.00ml, is placed in 100ml brown volumetric flask, adds water to be settled to scale, shakes up, obtain final product working solution,
The standard working solution of vitamin B1, B2, B3, B5, B6, B7, B12 is pressed embodiment 1 condition replication 6 times, Calculate its peak area RSD (%).Result such as table 3:
Table 3:Precision
Vitamin B1,6 peak areas of B2, B3, B5, B6, B7, B12 replication RSD be respectively 0.5%, 0.8%, 0.7%th, 0.8%, 0.6%, 0.7%, 0.7%, show that the method has preferable precision.
Embodiment 3
Precision weighs sample powder 180mg of vitamin B complex slow releasing tablet in 6 parts of multivitamin slow releasing capsule, is placed in 50ml In centrifuge tube, accurate addition 50.00ml water ultrasonic agitation dissolving, about 30min, let cool to room temperature, 8000r/min is centrifuged 5min, Through 0.22 μm of aqueous phase membrane filtration, obtain final product mensure test liquid.Sample introduction 2 μ l, by embodiment 1 testing conditions detection sample content,
Sample size computing formula is:
X=C × V/M × K
In formula:The content of vitamin B1, B2, B3, B5, B6, B7, B12, g/100g in X sample;
The quality of M sample, g;
K unit conversion factor (K=0.0001);
The extension rate of V sample, ml;
The concentration of vitamin B1, B2, B3, B5, B6, B7, B12 in C sample solution, μ g/ml.
Note:Calcium pantothenate changes into the coefficient 0.92 of pantothenic acid, need to be multiplied by when calculating pantothenic acid contrast solution concentration.
Calculate its peak area RSD (%).Result such as table 4:
Table 4 repeatability
6 parts of sample vitamin B1s, the RSD of B2, B3, B5, B6, B7, B12 content are respectively 0.7%, 0.8%, 0.9%, 0.8%th, 0.8%, 0.6%, 0.7%, show that the method has preferable repeatability, meet GB/T27404-2008《Laboratory matter Amount controls specification》Requirement【GB/T27404-2008 requires RSD (%)≤2.7%】.
Embodiment 4
Accurate absorption thiamine nitrate storing solution 3.00ml respectively, riboflavin storing solution 3.00ml, nicotiamide storing solution 20.00ml, calcium pantothenate storing solution 6.00ml, pyridoxine hydrochloride storing solution 3.00ml, biotin storing solution 1.00ml, cobalamine stores up Standby liquid 1.00ml, is placed in 100ml brown volumetric flask, adds water to be settled to scale, shakes up, obtain final product working solution.To work molten After liquid places 0h, 1h, 2h, 4h, 8h, 12h respectively at room temperature, measure peak area by embodiment 1 testing conditions, calculate its RSD (%).Result such as table 5:
Table 5 stability
Vitamin B1, B2, B3, B5, B6, B7, B12 standard working solution place at room temperature respectively 0h, 1h, 2h, 4h, After 8h, 12h, RSD be respectively 0.5%, 0.7%, 0.7%, 0.6%, 0.6%, 0.7%, 0.7%, show vitamin B1, B2, B3, B5, B6, B7, B12 standard working solution having good stability in 12 hours at room temperature.
Embodiment 5
Take pure water as detection sample, by pure water after ultrasonic 30min, through 0.22 μm of aqueous phase membrane filtration, that is, Obtain the test liquid of release completely.Sample introduction 2 μ l.During with vitamin B1, the appearance of B2, B3, B5, B6, B7, B12 standard working solution Between contrast.Result such as Fig. 8~14.
Result shows, blank solution equal no peak at vitamin B1, the appearance time of B2, B3, B5, B6, B7, B12, shows Blank substantially noiseless to measurement result.
Embodiment 6
Analysis method detection limit is calculated by signal to noise ratio (S/N).When signal to noise ratio (S/N) is 3, detection is limited to vitamin B1: 0.62937ng/ml;Vitamin B2:0.63612ng/ml;Vitamin B3:4.01198ng/ml;Vitamin B5:1.28751ng/ ml;Vitamin B6:0.63057ng/ml;Vitamin B7:10.49780ng/ml;Vitamin B12:10.69770ng/ml.
Embodiment 7
Mark-on:Precision weighs 9 parts of about 0.18g sample (vitamin B1 of known sample, B2, B3, B5, B6, B7, B12 content It is respectively:1.215%th, 1.066%, 11.948%, 2.732%, 1.218%, 0.528%, 2.526mg/100g), it is divided into 3 Group, every group 3 parts, each group accurate addition thiamine nitrate respectively, riboflavin, nicotiamide, calcium pantothenate, pyridoxine hydrochloride, biotin, Appropriate cobalamine.
Testing sample is placed in 50ml centrifuge tube, accurate addition 50.00ml water ultrasonic agitation dissolving, about 30min, lets cool To room temperature, 8000r/min is centrifuged 5min, through 0.22 μm of aqueous phase membrane filtration, sample introduction 2 μ l.Measure by embodiment 1 testing conditions Peak area, calculates its RSD (%).
Record addition=mark-on sample measured amount-sample measured amount
The response rate (%)=record addition/theoretical addition amount
Result such as table 6:
Table 6 response rate
Vitamin B1, the average recovery rate of B2, B3, B5, B6, B7, B12 are respectively:99.1%th, 99.3%, 99.3%, 99.8%th, 100.1%, 99.3%, 99.5%, relative standard deviation (RSD) be respectively 0.8%, 0.7%, 0.8%, 0.6%, 0.6%th, 0.6%, 0.5%, meet GB/T27404-2008《Good Laboratory controls specification》Requirement【GB/T27404-2008 The response rate is required to be 95 105%】.
By the content assaying method of vitamin B1, B2, B3, B5, B6, B7, B12 is carried out linearly, precision, repetition Property, stability, blank, detection limit, recovery test, all meet GB/T27404-2008《Good Laboratory controls specification》Will Ask it was demonstrated that content assaying method scientific and effective, can to the vitamin B1 of multivitamin slow releasing capsule, B2, B3, B5, B6, B7, B12 content plays the purpose of quality control.
The above is only the preferred embodiment of the present invention it is noted that coming for those skilled in the art Say, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should be regarded as Protection scope of the present invention.

Claims (10)

1. a kind of detection method of vitamin B group is it is characterised in that with aqueous formic acid or acetic acid aqueous solution for mobile phase A phase; With methanol or acetonitrile for Mobile phase B phase;Using High performance liquid chromatography mass spectrometry, sample is detected, according to mass spectrum and Chromatogram carries out qualitative and/or quantitative to vitamin B group;
Described high performance liquid chromatography adopts gradient elution, and elution program is:
0~0.5min, the volume fraction of mobile phase A phase is 92%;
0.5min~8min, the volume fraction of mobile phase A phase is down to 10% by 92%;
8min~8.5min, the volume fraction of mobile phase A phase is 10%;
8.5min~9min, the volume fraction of mobile phase A phase rises to 92% by 10%;
9min~12min, the volume fraction of mobile phase A phase is 92%.
2. detection method according to claim 1 is it is characterised in that in described aqueous formic acid, the volume fraction of formic acid For 0.1%;In described acetic acid aqueous solution, the volume fraction of acetic acid is 0.1%.
3. detection method according to claim 1 is it is characterised in that the flow velocity of described mobile phase of high performance liquid chromatography is 0.3mL/min~0.5mL/min.
4. detection method according to claim 1 is it is characterised in that the column temperature of the chromatographic column of described high performance liquid chromatography is 30 DEG C~40 DEG C.
5. detection method according to claim 1 is it is characterised in that the chromatographic column of described high performance liquid chromatography is C18 color Spectrum post, a size of 100 × 4.6mm, 2.6 μm;150 × 4.6mm, 2.7 μm or 100 × 4.6mm, 3 μm.
6. detection method according to claim 1 is it is characterised in that described mass spectrographic ion source is electron spray cation Source;Ion source temperature is 600 DEG C.
7. detection method according to claim 1 is it is characterised in that described mass spectrographic electron spray voltage is 5500V;Collision Air pressure 7.0psi;Gas curtain air pressure 22.0psi;Atomization air pressure 60.0psi;Secondary air speed 20.0psi.
8. detection method according to claim 1 is it is characterised in that described sample is through pre-treatment, the side of described pre-treatment Formula is:Supersound extraction is carried out for solvent to the sample after pulverizing with water, filtration sterilization after centrifugation;The time of described supersound extraction For 20min~40min;Temperature is 10 DEG C~30 DEG C, and power is 0.8kW~1.1kW, and frequency is 37kHz~45kHz.
9. the application in the vitamin B group detection in health product of the detection method described in any one of claim 1~8.
10. application according to claim 9 is it is characterised in that described health product are multivitamin slow releasing capsule.
CN201610882137.3A 2016-10-09 2016-10-09 Method for detection of B vitamins Pending CN106442790A (en)

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Cited By (4)

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CN104914192A (en) * 2015-06-30 2015-09-16 华润紫竹药业有限公司 Analytical method of multivitamin tablets
CN109444293A (en) * 2018-12-26 2019-03-08 中国烟草总公司郑州烟草研究院 The detection method of endogenous water-soluble B vitamin in a kind of fresh tobacco leaves
CN110412186A (en) * 2019-07-16 2019-11-05 上海康识食品科技有限公司 Vitamin B in a kind of measurement condensed food1And vitamin B2Method
CN114137116A (en) * 2021-11-29 2022-03-04 江苏知原药业股份有限公司 Method for detecting content of nicotinamide in metronidazole gel

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