CN107831231A - A kind of method for detecting vitamin A impurity in multivitamin preparation - Google Patents
A kind of method for detecting vitamin A impurity in multivitamin preparation Download PDFInfo
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- CN107831231A CN107831231A CN201711054538.0A CN201711054538A CN107831231A CN 107831231 A CN107831231 A CN 107831231A CN 201711054538 A CN201711054538 A CN 201711054538A CN 107831231 A CN107831231 A CN 107831231A
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Abstract
The invention discloses a kind of method for detecting vitamin A impurity in multivitamin preparation, methods described comprises the following steps, chromatographic condition：Chromatographic column：Using octadecylsilane chemically bonded silica as filler；Using methanol absolute ethyl alcohol as mobile phase；Detection wavelength：300~350nm；Column temperature：20~50 DEG C；Flow velocity：0.5~2.0mL/min；Sample size：10~200 μ l；Run time：50~150 minutes.It is prepared by sample solution：Take this product content to be dissolved in dichloromethane, wash, take a layer solution, dilute, centrifugation, subsequent filtrate separately takes need testing solution dilution to be used as contrast solution as need testing solution.Measure：Above-mentioned solution is injected separately into liquid chromatograph, record chromatogram measure.The testing cost of the present invention is low, mobile phase safety, and specificity is strong, easy to operate, the content and impurity of vitamin A in the multivitamin preparation detected containing vitamin A that can be rapidly and efficiently, effectively controls the quality of multivitamin preparation.
Description
Technical field
The present invention relates to a kind of method for detecting vitamin A impurity in multivitamin preparation in Pharmaceutical Analysis field.
Background technology
Vitamin A is fat-soluble alcohols material, is the vitamin being found earliest, and vitamin A has different kinds of molecules form,
Its entitled retinol of chemistry, its main Physiological Function have (1) to maintain normal vision function；(2) Epithelial cell is safeguarded
Health and the synthesis for promoting immunoglobulin；(3) bone normal growth and development is maintained；(4) growth and reproduction are promoted；(5) suppress
Tumour growth；(6) nutritional supplement.In addition, vitamin A is additionally aided to the disease such as acne, useless fellow, furuncle sore, skin surface ulcer
Treatment；Contribute to the treatment to pulmonary emphysema, hyperthyroidism；Contribute to hair growth and help to dispel old age
Spot.Therefore, when human body is deficient in vitamin A, eye symptom has：Yctalopia, Bitot's spots, xeroma；Skin symptom is：Skin
Skin is easily dried, angling hyperplasia, furfur.
In view of numerous functions of vitamin A, the quality research of vitamin A is most important in multivitamin preparation, dimension life
Plain A includes Retinol Palmitate and vitamine A acetate.Because Retinol Palmitate chemical property is stable and is not easy point
Solution, therefore Retinol Palmitate is selected in invention formulation as raw material.Though there is document report Retinol Palmitate miscellaneous
The assay method of matter, but it is miscellaneous to be directed to vitamin A in the compound preparation being made up of multivitamin there has been no document and patent at present
The report of quality detection method, this method is more sensitive convenient in need testing solution preparation, experimental implementation etc., has filled up a variety of
The blank of vitamin A method for detecting impurities in the compound preparation of vitamin composition, this method specificity, reappearance are good, can
Fast and effectively separation determination goes out vitamin A impurity in multivitamin preparation, can effectively control the matter of multivitamin preparation
Amount.
The content of the invention
It is an object of the invention to provide a kind of operation is simpler and more direct, sensitivity is higher, the multivitamin system of favorable reproducibility
The detection method of vitamin A content and impurity in agent.Methods described includes：
Multivitamin preparation containing vitamin A is configured to detection solution by pre-treatment, with octadecylsilane key
Conjunction silica gel is chromatographic column, using methanol-absolute ethyl alcohol mobile phase, record HPLC figures.
Preferably, the detection solution manufacturing method is：Take this product content appropriate, it is molten to add 5~30ml of dichloromethane
Solution, add water washing 1~5 time, discard water layer, take dichloromethane layer solution, add absolute ethyl alcohol be diluted in every milliliter of solution containing about
Vitamin A is 1~100 μ g solution, and centrifugation, subsequent filtrate is as need testing solution.It is another to take need testing solution, absolute ethyl alcohol dilution
100 times, as contrast solution.
Preferably, the extractant during prepared by the need testing solution is dichloromethane；It is dilute in reference substance solution preparation
It is absolute ethyl alcohol to release agent.
Preferably, the mobile phase is the proportioning solution of methanol-absolute ethyl alcohol.
Preferably, the column temperature is 20~50 DEG C；
Preferably, the flow velocity of the mobile phase is 0.5~2.0mL/min.
Preferably, the chromatographic column is octadecylsilane chemically bonded silica.
Preferably, the Detection wavelength is 300~350nm.
The present invention is characterized by the trial-manufacture of sample method of our uniquenesses and efficiently quickly determines a variety of dimensions using HPLC methods
The content and impurity of vitamin A in raw plain preparation.This method specificity is strong, favorable reproducibility, high sensitivity, and is flowed in the present invention
Mutually simple nontoxic, testing cost is low, safe and reliable, can be widely used in Pharmaceutical Analysis field, contains so as to better assure that
The quality and validity of the multivitamin preparation of vitamin A.
Brief description of the drawings
Fig. 1：In embodiment 1 in multivitamin preparation vitamin A impurity determination negative sample collection of illustrative plates
Fig. 2：In embodiment 1 in multivitamin preparation vitamin A impurity determination reference substance collection of illustrative plates
Fig. 3：In embodiment 1 in multivitamin preparation vitamin A impurity determination test sample collection of illustrative plates
Fig. 4：Vitamin A impurity determination collection of illustrative plates in multivitamin preparation in embodiment 2
Fig. 5：Vitamin A impurity determination collection of illustrative plates in multivitamin preparation in embodiment 3
Fig. 6：Vitamin A impurity determination collection of illustrative plates in multivitamin preparation in embodiment 4
Embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described,
Obviously, described embodiment is only part of the embodiment of the present invention, rather than whole embodiments.Based in the present invention
Embodiment, the every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made, all
Belong to the scope of protection of the invention.
Embodiment 1
1st, chromatographic condition
Instrument：High performance liquid chromatograph；
Chromatographic column：DiKMAC18Post (model：Diamonsil, 250 × 4.6mm, 5 μm)；
Mobile phase：Methanol-absolute ethyl alcohol (52:48)；
Detection wavelength：324nm；
Column temperature：20℃；
Flow velocity：1.0ml/min；
Run time：About 70 minutes
2nd, sample preparation
(1) preparation of mobile phase
Precision measures methanol 520ml and absolute ethyl alcohol 480ml, mixes, and it is 52 to produce 1000ml proportionings:48 methanol-nothing
Water-ethanol mobile phase.
(2) prepared by need testing solution
It is appropriate (being approximately equivalent to the unit of vitamin 5000) to weigh this product content, it is accurately weighed, put in separatory funnel, it is accurate
Dichloromethane 10ml dissolvings are added, adds water washing 2 times, each 10ml, discards water layer, precision measures dichloromethane layer solution 2ml,
Put in 25ml measuring bottles, add absolute ethyl alcohol to be diluted to scale, shake up, centrifugation (3000 turns per minute) 10 minutes, take supernatant, filter
Cross, take subsequent filtrate as need testing solution.
(3) prepared by reference substance solution
Precision measures need testing solution 1ml, puts in 100ml measuring bottles, adds absolute ethyl alcohol to be diluted to scale, molten as compareing
Liquid.
(5) experimental result
If any impurity peaks in the chromatogram of need testing solution, the negative peak (auxiliary material before relative retention time 0.55 is deducted
Peak and other drugs are into swarming) and solvent peak calculated.This method can effectively detect the multivitamin system containing vitamin A
Vitamin A content in agent.Collection of illustrative plates is shown in Fig. 1,2,3 of Figure of description.
Embodiment 2
Instrument：High performance liquid chromatograph；
Chromatographic column：DiKMAC18Post (model：Diamonsil, 250 × 4.6mm, 5 μm)；
Mobile phase：Methanol-absolute ethyl alcohol (52:48)；
Detection wavelength：315nm；
Column temperature：30℃；
Flow velocity：1.5ml/min；
Run time：About 70 minutes
Solution compound method and assay method are carried out according to the method for " sample solution preparation " in embodiment 1, as a result see Fig. 4.
Embodiment 3
Instrument：High performance liquid chromatograph；
Chromatographic column：DiKMAC18Post (model：Diamonsil, 250 × 4.6mm, 5 μm)；
Mobile phase：Methanol-absolute ethyl alcohol (50:50)；
Detection wavelength：330nm；
Column temperature：25℃；
Flow velocity：0.8ml/min；
Run time：About 70 minutes
Solution compound method and assay method are carried out according to the method for " sample solution preparation " in embodiment 1, as a result see Fig. 5.
Embodiment 4
Instrument：High performance liquid chromatograph；
Chromatographic column：DiKMAC18Post (model：Diamonsil, 250 × 4.6mm, 5 μm)；
Mobile phase：Methanol-absolute ethyl alcohol (54:46)；
Detection wavelength：325nm；
Column temperature：35℃；
Flow velocity：1.2ml/min；
Run time：About 70 minutes
Solution compound method and assay method are carried out according to the method for " sample solution preparation " in embodiment 1, as a result see Fig. 6.
Embodiment 5
1. material solution：Vitamin A raw material about 10mg is taken, is dissolved with dichloromethane, absolute ethyl alcohol dilution is made every 1ml and contained
0.02mg solution, shakes up, and filtering, produces.
2. need testing solution：This product content about 2.0g is taken, according to " the need testing solution preparation method under the item of embodiment 1 "
Prepare, produce.
3. negative solution：Vitamin A negative sample (part for being free of vitamin A) about 2g is taken, is prepared with need testing solution,
Produce.
4. auxiliary material solution：Right amount of auxiliary materials is taken, prepares, produces with need testing solution.
5. contrast solution：Precision measures 1ml need testing solutions, puts in 100ml volumetric flasks, adds absolute ethyl alcohol to be diluted to quarter
Degree, shakes up, produces.
Precision measures above-mentioned test sample, corresponding negative sample solution, contrast solution and blank auxiliary solution each 100 respectively
μ l, inject liquid chromatograph, analysis result.
The sample specificity result of the test of table 1
The peak purity result of the test of table 2
As a result show：Test sample does not produce other new impurity under each failure condition, shows that vitamin A is relatively stable.
Under this chromatographic condition, vitamin A main peak can efficiently separate with producing impurity after forced degradation in test sample, color
Spectral peak purity is high, foreign body is not detected by, available for this product vitamin A Related substances separation.
As seen from the figure, under the chromatographic condition, blank auxiliary and negative sample solution are to the relevant material of this product vitamin A
Measure is noiseless, and the negative peak before simply should deducting relative retention time 0.55 when calculating test sample about material is (auxiliary
Expect peak and other drugs into swarming) and solvent peak.
Claims (6)
- A kind of 1. method for detecting vitamin A impurity in multivitamin preparation, it is characterised in that methods described includes following step Suddenly：（1）Chromatographic condition：With C18For chromatographic column；Using methanol-absolute ethyl alcohol as mobile phase；Detection wavelength：300~350nm；Column temperature： 20~50 DEG C；Flow velocity：0.5~2.0mL/min；Sample size：10~200 μ l, run time 50~150 minutes；（2）Sample solution Preparation：Take this product content appropriate, add 5~30ml of dichloromethane dissolvings, add water washing 1~5 time, 5~50ml, is abandoned every time Water layer is removed, takes dichloromethane layer solution, it is the molten of 1~100 μ g to add absolute ethyl alcohol to be diluted in every milliliter of solution containing about vitamin A Liquid, centrifugation, subsequent filtrate is as need testing solution；Another to take need testing solution, absolute ethyl alcohol dilutes 100 times, as contrast solution； （3）Measure：Above-mentioned solution is injected into high performance liquid chromatograph, chromatogram is recorded and is analyzed.
- 2. according to the method for claim 1, it is characterised in that the chromatographic column is using octadecylsilane chemically bonded silica to fill out Material, its granularity are 3 μm, 5 μm, 7 μm or 10 μm；Its internal diameter is 2~5mm；Its length is 10~30cm.
- 3. according to the method for claim 1, it is characterised in that the mobile phase for nonpoisonous organic solvent methanol-anhydrous Ethanol, ratio 52:48.
- 4. the preparation of need testing solution according to claim 1, it is characterised in that the organic solvent be dichloromethane or Chloroform.
- 5. the preparation of need testing solution according to claim 1, it is characterised in that the rotating speed centrifuged in the experiment is every 1500~5000 turns of minute, time are 5~50 minutes.
- 6. the preparation of reference substance solution according to claim 1, it is characterised in that the reference substance uses nothing for test sample Water-ethanol dilutes 100 times of gained.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109239230A (en) * | 2018-10-30 | 2019-01-18 | 广州汉光药业股份有限公司 | The impurity analysis method of multivitamin preparation |
| CN110715995A (en) * | 2018-07-12 | 2020-01-21 | 北京藏卫信康医药研发有限公司 | Method for detecting impurities of multi-vitamin injection |
| CN114437093A (en) * | 2021-11-11 | 2022-05-06 | 浙江新和成股份有限公司 | Identification and extraction method of impurity A in aromatization reaction liquid of vitamin B6 and synthesis method of impurity A |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110715995A (en) * | 2018-07-12 | 2020-01-21 | 北京藏卫信康医药研发有限公司 | Method for detecting impurities of multi-vitamin injection |
| CN110715995B (en) * | 2018-07-12 | 2023-11-03 | 北京藏卫信康医药研发有限公司 | Method for detecting impurities of multivitamin injection |
| CN109239230A (en) * | 2018-10-30 | 2019-01-18 | 广州汉光药业股份有限公司 | The impurity analysis method of multivitamin preparation |
| CN114437093A (en) * | 2021-11-11 | 2022-05-06 | 浙江新和成股份有限公司 | Identification and extraction method of impurity A in aromatization reaction liquid of vitamin B6 and synthesis method of impurity A |
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Application publication date: 20180323 |