CN103728385B - A kind of method of fosfomycin sodium in use chromatography of ions detection pharmacy waste water - Google Patents
A kind of method of fosfomycin sodium in use chromatography of ions detection pharmacy waste water Download PDFInfo
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- CN103728385B CN103728385B CN201310719495.9A CN201310719495A CN103728385B CN 103728385 B CN103728385 B CN 103728385B CN 201310719495 A CN201310719495 A CN 201310719495A CN 103728385 B CN103728385 B CN 103728385B
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Abstract
The present invention relates to the method for fosfomycin sodium in a kind of use chromatography of ions detection pharmacy waste water, it the described method comprises the following steps：(1) chromatographic condition：Chromatographic column is low capacity hydroxyl system cathodic protection post and high power capacity anion exchange separation column, and suppressor is using the membrane suppressor of electrolysis, and electric conductivity detector, leacheate is potassium salt soln；(2) to the preparation of standard liquid：The standard items of fosfomycin sodium are taken to be configured to standard solution with ultra-pure water；(3) pre-treatment of sample：For detection sample with after 0.45 μm of membrane filtration after C18 pillars remove water sample in organic matter；(4) assay method：Take standard liquid to inject ion chromatograph, record spectrogram, determine standard peak position, calculate the area at fosfomycin sodium peak, standard curve is drawn according to gained peak area is calculated；Test sample is taken, ion chromatograph is injected, spectrogram is recorded, the concentration of sample is gone out according to the areal calculation at fosfomycin sodium peak.The present invention has the favorable reproducibility detected to fosfomycin sodium in pharmacy waste water, detection limit is low, sensitivity is high, simple to operate, testing conditions are gentle, test facilities and instruments is widely used, the advantages of source of leacheate potassium salt soln is wide, configuration is simple, will be widely used in the detection of fosfomycin sodium in industrial wastewater.
Description
Technical field
The invention belongs to compound test field, the method for relating more specifically to detect fosfomycin sodium in pharmacy waste water.
Technical background
Phosphonomycin (Fosfomysin, FOM), chemical name (1R, 2S) -1,2- phosphate epoxypropyls is a kind of new wide
Compose antibiotic.Phosphonomycin can effectively suppress phosphoenolpyruvate transferase to suppress the synthesis of mucopeptide, blue to most leather
Family name's positive bacteria, negative bacterium all have killing action, currently without discovery cross resistance its clinic are gradually increased, industry
Production scale also gradually increases.
Phosphonomycin is a kind of highly polar micromolecular compound, and molecular weight is 138, more than at 220nm without UV absorption, because
And in Pharmaceutical Analysis field, the separation analysis of phosphonomycin is also a great problem always.It is main with its sodium salt in industrial production
Or the form production application of calcium salt.For sterling fosfomycin sodium, mainly determined using the Microbiological methods in Chinese Pharmacopoeia
The potency of sterling fosfomycin sodium.This method has the advantages that pre-treatment is simple, economical, of large quantities, but sensitivity it is relatively low, it is time-consuming compared with
Long, operation is more complicated, is vulnerable to the interference of other antibiotic, often lacks selectivity and accuracy, and the method is simultaneously of little use.
Usual phosphonomycin is made by chemical synthesis process, and it produces waste water and contains substantial amounts of organic pollution (as instead
Answer raw material, phosphonomycin analogue, intermediate product etc.), composition is complicated, further increases the difficulty of detection.
CN102841155A Chinese patent literatures disclose a kind of use to be had in high performance liquid chromatography detection fosfomycin sodium
The method for closing material.This method is used for the content for testing fosfomycin sodium in fosfomycin sodium sterling, and this method of testing is matched somebody with somebody in solution
System, detection process all have certain advantage, but detect fosfomycin sodium from waste water, and be still significantly improved space.
The content of the invention
In view of the above-mentioned problems, the present invention sets about from the recycling two of wastewater treatment and resource in terms of, research is a kind of efficient,
Quickly, the method for detecting fosfomycin sodium in pharmacy waste water of low detection limits.
It is an object of the invention to：The method that fosfomycin sodium in a kind of use chromatography of ions detection pharmacy waste water is provided.
The present invention main technical schemes be：A kind of method of fosfomycin sodium in use chromatography of ions detection pharmacy waste water,
Comprise the following steps：
(1) chromatographic condition：Chromatographic column is low capacity hydroxyl system cathodic protection post and high power capacity anion exchange separation
Post, suppressor is using the membrane suppressor of electrolysis, and electric conductivity detector, leacheate is potassium salt soln；
(2) to the preparation of standard liquid：The standard items of fosfomycin sodium are taken to be configured to reference substance solution with ultra-pure water；
(3) pre-treatment of sample：For detection sample with after 0.45 μm of membrane filtration after C18 pillars remove water sample in
Organic matter.
(4) assay method：Take standard liquid to inject ion chromatograph, record spectrogram, determine standard peak position, calculate phosphorus mould
The area at plain sodium peak, standard curve is drawn according to gained peak area is calculated；Test sample is taken, ion chromatograph, record spectrum is injected
Figure, the concentration of sample is gone out according to the areal calculation at fosfomycin sodium peak.
In above-mentioned method of testing, the pore diameter range of the miillpore filter of the filtering fosfomycin sodium waste water is not higher than 0.45 μ
m；
In above-mentioned method of testing, the standard items of fosfomycin sodium are configured to standard solution with ultra-pure water, and concentration range is 0-
20mg/L.
In above-mentioned method of testing, the chromatographic column is Dionex IonPacTMAG11-HC cathodic protections post and Dionex
IonPacTMAS11-HC anion columns, the suppressor is ASRS300, and the detector is electric conductivity detector, the leacheate
For 20-40mmol KOH, preferably 30mmol；The electric current 60-80mA, preferably 75mA；The flow velocity is 0.5-1.5ml/
Min, preferably 1.0ml/min,；25-35 DEG C of the column temperature, preferably 30 DEG C.
In above-mentioned method of testing, described standard items and the sampling volume of sample are 10-40 μ L, preferably 25 μ L.
In above-mentioned method of testing, the minimum detectability of fosfomycin sodium is 0.06mg/L in pharmacy waste water.
The present invention is characterized by the method that fosfomycin sodium in pharmacy waste water is detected using chromatography of ions.Its principle is：Profit
With fosfomycin sodium and the difference of impurity design feature, by the chromatography of ions, using low capacity hydroxyl system cathodic protection post
With high power capacity anion exchange separation column as chromatographic column, KCl solution is leacheate so that fosfomycin sodium and impurity are obtained well
Separation, then is detected by the membrane suppressor and electric conductivity detector of electrolysis, so as to obtain containing for fosfomycin sodium in pharmacy waste water
Amount.
The present invention use chromatography of ions detection pharmacy waste water in fosfomycin sodium method compared with prior art, with pair
Fosfomycin sodium is detected in pharmacy waste water favorable reproducibility, detection limit is low, sensitivity is high, simple to operate, testing conditions gentle, detection
Extensively, the source of leacheate potassium salt soln is wide, the advantages of configure simple, can be widely applied to industrial wastewater for equipment and instrument application
The detection of middle fosfomycin sodium.
Brief description of the drawings
Accompanying drawing 1 is the chromatography of ions schematic diagram of the Plays product of case study on implementation 1.
Accompanying drawing 2 is the standard curve of the fosfomycin sodium of case study on implementation 1.
Accompanying drawing 3 is the chromatography of ions schematic diagram of the pharmacy waste water of case study on implementation 1.
Embodiment
The method of the present invention is explained further by the following examples, still, implementation of the invention is not limited to following form.
Embodiment 1：
Chromatographic condition
Chromatographic column：Dionex IonPacTMAG11-HC cathodic protections post (50 × 4mm) and Dionex IonPacTM
AS11-HC anion columns (250 × 4mm)；
Detector：ASRS300, electric conductivity detector, electric current 75mA；
Leacheate：30mmol KCl, flow velocity is 1.0ml/min；
Detector temperature：30℃.
(1) standard items are configured
It is 9.60mg mL with ultra-pure water configuration concentration to take the standard items of fosfomycin sodium first-1Fosfomycin sodium standard reserving solution,
Be 1 according still further to required concentration configuration concentration, 2,5,8,10,12,16mg/L standard liquid.
(2) preparation of samples
Sample for detection produces the production waste water of fosfomycin sodium from chemical synthesis, using 0.45 μm of filter membrane mistake
Filter, then the organic matter in water sample is removed by C18 pillars；
(3) sample detection
Take 1,2,5,8,10,12,16mg/L standard liquid samples, after distinguishing sample introduction, the μ L of sample size 25, note after instrument stabilizer
Spectrogram is recorded, determines that fosfomycin sodium standard items appearance time is 3.847min according to spectrogram, fosfomycin sodium peak is calculated with integration method
Area as shown in table 1, is drawn shown in standard curve according to concentration of standard solution and corresponding peak area, and obtains matched curve and be
Y=20.4082x-0.1224 (y is concentration, and x is peak area)；3, fosfomycin sodium pharmacy waste water sample is taken, each sample is parallel
The pin of sample introduction 10, the μ L of sample size 25 record spectrogram, the area at fosfomycin sodium peak are calculated with integration method, by the area at fosfomycin sodium peak
The concentration that y=20.4082x-0.1224 calculates sample is substituted into, as a result as shown in table 2
The standard curve of 1 embodiment of table 1
| Concentration | Peak area (μ s*min) |
| 1 | 0.0461 |
| 2 | 0.0919 |
| 5 | 0.2369 |
| 8 | 0.3803 |
| 10 | 0.4906 |
| 16 | 0.7313 |
The result of 2 embodiment of table 1
| Sample | Pharmacy waste water (mg L-1) |
| Sample 1 | 0.43 |
| Sample 2 | 0.43 |
| Sample 3 | 0.45 |
| Average value | 0.43 |
| Standard deviation | 0.02 |
| Relative standard deviation (RSD) | 0.04 |
Claims (7)
1. the method for fosfomycin sodium, the described method comprises the following steps in a kind of use chromatography of ions detection pharmacy waste water：
Chromatographic condition：
Chromatographic column is low capacity hydroxyl system cathodic protection post and high power capacity anion exchange separation column, and suppressor is using electrolysis
Membrane suppressor, electric conductivity detector, leacheate be 30mmol KCl solution；
(1) to the preparation of standard liquid
The standard items of fosfomycin sodium are taken to be configured to standard solution with ultra-pure water；
(2) pre-treatment of sample
Sample for detection removes the organic matter in water sample using 0.45 μm of membrane filtration, then by C18 pillars；
(3) sample is determined
Take standard liquid to inject ion chromatograph, record spectrogram, determine standard peak position, calculate the area at fosfomycin sodium peak, root
Standard curve is drawn according to gained peak area is calculated；Test sample is taken, ion chromatograph is injected, spectrogram is recorded, according to fosfomycin sodium
The areal calculation at peak goes out the concentration of sample.
2. the method for fosfomycin sodium in use chromatography of ions detection pharmacy waste water according to claim 1, it is characterised in that：
The chromatographic column is Dionex IonPacTMAG11-HC cathodic protections post and Dionex IonPacTMAS11-HC anion
Post, the suppressor is ASRS300, and the detector is electric conductivity detector, and the leacheate is 20-40mmol KCl；It is described
Electric current 60-80mA；The flow velocity is 0.5-1.5ml/min；The column temperature is 25-35 DEG C.
3. the method for fosfomycin sodium in use chromatography of ions detection pharmacy waste water according to claim 2, it is characterised in that：
The leacheate is 30mmol KCl；The electric current 75mA；The flow velocity is 1.0ml/min；The column temperature is 30 DEG C.
4. the method for fosfomycin sodium in use chromatography of ions detection pharmacy waste water according to claim 1, it is characterised in that：
In step (1), the concentration of fosfomycin sodium is 0-20mg/L in described standard liquid.
5. the method for fosfomycin sodium in use chromatography of ions detection pharmacy waste water according to claim 1, it is characterised in that：
In step (3), described standard items and the sampling volume of sample are 10-40 μ L.
6. the method for fosfomycin sodium in use chromatography of ions detection pharmacy waste water according to claim 1, it is characterised in that：
Described standard items and the optimal sampling volume of sample are 25 μ L.
7. the method for fosfomycin sodium in use chromatography of ions detection pharmacy waste water according to claim 1, it is characterised in that：
The minimum detectability of fosfomycin sodium is 0.06mg/L in pharmacy waste water.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102128885B (en) * | 2010-12-08 | 2013-01-30 | 广东中烟工业有限责任公司 | Method for quickly and simultaneously detecting 16 inorganic anions and organic acids in tobacco |
| CN102798681A (en) * | 2012-08-17 | 2012-11-28 | 红云红河烟草(集团)有限责任公司 | Method for determining nitrate and nitrite ions in cigarette tipping paper |
| CN102841155B (en) * | 2012-09-25 | 2014-11-26 | 东北制药集团股份有限公司 | Method for detecting related substances in fosfomycin sodium by high-performance liquid chromatography |
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