CN102230920A - Determination method of polymyxins E residue content in animal source food by superhigh liquid chromatogram-tandom mass spectrometry - Google Patents
Determination method of polymyxins E residue content in animal source food by superhigh liquid chromatogram-tandom mass spectrometry Download PDFInfo
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- CN102230920A CN102230920A CN2011100729770A CN201110072977A CN102230920A CN 102230920 A CN102230920 A CN 102230920A CN 2011100729770 A CN2011100729770 A CN 2011100729770A CN 201110072977 A CN201110072977 A CN 201110072977A CN 102230920 A CN102230920 A CN 102230920A
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Abstract
The invention relates to a determination method of polymyxins E residue content in animal source food by superhigh liquid chromatogram-tandom mass spectrometry. The method comprises the following steps: adding an extract in a sample to be measured, fully whirling and extracting, high-speed freezing and centrifuging, then obtaining a sample liquid after filtering and purifying; weighing a polymyxins E standard sample, dissolving by methanol to take it as a storing solution, then further, diluting by methanol to obtain a standard working solution possessing a concentration gradient; detecting the sample by using a superhigh liquid chromatogram-tandom quadrupole liquid chromatography-mass spectrometer; reading out the concentration value of polymyxins E on a standard curve, and calculating the result of polymyxins E of the sample. According to the invention, the determination method of polymyxins E residue in animal source food is rapid and effective, the relative average deviation is less than 10%. Therefore, the method provided in the invention is reliable and easy to enforce for detecting polymyxins E residue in animal source food, which is capable of satisfying the requirments of research and production.
Description
The assay method of polymyxin e residual quantity
Technical field
The present invention relates to the assay method of polymyxin e residual quantity in the animal derived food, particularly relate to a kind of method that the residual quantity of polymyxin e in the animal derived food is detected by Ultra Performance Liquid Chromatography-tandem mass spectrometer.
Background technology
Polymyxins belongs to polypeptide antibiotics, mainly contains A, B, C, D, five kinds of compositions of E.What veterinary clinic was used mainly is polymyxin B, polymyxin e, and wherein with polymyxin B, antibacterial activity is the strongest, but its toxicity is bigger.And polymyxin e is a colistin, has lower toxicity and good antibiotic vigor.Polymyxin e is that Koyama etc. is separated to a strain bacillus polymyxa colistin and becomes the basic polypeptide class microbiotic that produces in the strain nutrient solution from Fukushima county soil.Polymyxin e has another name called colistin, Ke Lisiting, colistin, colistin etc., it is a kind of mixture that contains more than 30 kind of heterogeneity at least, be mainly the potpourri of Colistin A and Polymyxin E2, the molecular formula of colistin A and colistin B is respectively C
53H
100N
16O
13And C
52H
98N
16O
13In recent years, the multi-drug resistant of false bacillus and acinetobacter calcoaceticus appears in some countries, and polymyxins is treated this bacterioid and has better effects.But to reduce its toxic and side effect as far as possible, make full use of its growth promotion and prevention, therapeutic action; Avoid random escalated dose or prolongation administration time and cause unnecessary toxic and side effect; Behind the intramuscular injection colistin to there be the off-drug period; Forbid to use colistin in the livestock and poultry laying period and the phase of giving milk.Therefore set up a kind of quick, accurate, convenient and economic detection method, help the residual quantity of colistin in the monitor animal derived food.
Summary of the invention
Technical matters to be solved by this invention is, by groping the best proportioning of extract, and best extraction time, best purification condition and best chromatogram mass spectrum condition and the determination of residual amount method of polymyxin e in the animal derived food is provided.
For achieving the above object, the present invention takes following design proposal:
The assay method of polymyxin e residual quantity comprises the steps: in the animal derived food of the present invention
The sample 5.0g (being accurate to 0.0001g) that takes by weighing powder adds extract 25mL in 50mL tool plug centrifuge tube, behind the homogeneous 2min, and 4 ℃ of centrifugal 10min of following 10000r/min.Shift supernatant to another centrifuge tube, add the 20mL extract in the residue and repeat the above operation of extracting.Merge extract supernatant 2 times after, add normal hexane 20mL vortex 2min, the centrifugal 10min of 10000r/min discards upper strata liquid.Add normal hexane 20mL in the subnatant again and repeat above degreasing operation, the gained subnatant is to be clean.
Above-mentioned gained sample extract is transferred to Oasis HLB decontaminating column (with each the 6mL prewashing activation of first alcohol and water), uses the 10mL water washing earlier, discard effluent.Use the 3mL methanol-eluted fractions again, collect eluent, nitrogen flows down organic phase is dried up in 40 ℃ of water-baths.Behind 1.00mL, mixing through 0.22 μ m membrane filtration, obtains sample treatment solution to sample with dissolve with methanol and constant volume.
Take by weighing the polymyxin e standard items, with behind the dissolve with methanol as storing solution, further use liquid for standard then with concentration gradient with methyl alcohol dilution;
Utilize Ultra Performance Liquid Chromatography-tandem mass spectrometer that titer and sample treatment solution are detected;
Result of calculation, the computing formula of polymyxin e is in the sample:
In the formula:
The residual quantity of polymyxin e in the X-sample, unit is every kilogram of microgram (ug/kg);
The concentration of polymyxin e (ng/mL) in the C-sample treatment solution;
The final constant volume of V-sample extract, unit are milliliter (ml);
The sample weighting amount of m-sample, unit is gram (g);
Preferably, described extraction solvent is methyl alcohol and aqueous formic acid, and ratio is 10: 4.
Preferably, homogeneous extraction time is 2min.
Preferably, 10000r/min high speed refrigerated centrifuge 10.0min under 4 ℃ the condition.
Described Ultra Performance Liquid Chromatography-the tandem mass spectrometer that utilizes to the condition that sample treatment solution detects is:
Liquid phase chromatogram condition
Analytical column: Acquity BEH-C18,2.1mm * 50mm, 1.7 μ m
Moving phase: acetonitrile+0.1% aqueous formic acid=20+80
Flow velocity: 0.2mL/min.
Sample size: 10 μ L.
The mass spectrum condition
Ion gun: electric spray ion source;
Scan mode: positive ion scanning;
Detection mode: multiple-reaction monitoring;
Electron spray voltage: 3.0kv;
Ion source temperature: 110 ℃;
The temperature of desolvating: 400 ℃;
Ion pair, taper hole voltage, collision energy see Table 1.
The ion pair of table 1 polymyxin e, taper hole voltage, collision energy
And qualitative according to retention time, the external standard peak area method is quantitative.
Advantage of the present invention is: adopt method of the present invention to detect the assay method of polymyxin e residual quantity in the animal derived food, effectively, RSD detects and is limited to 25ug/kg less than 10% fast.This shows that method of the present invention be to detect the residual quantity of polymyxin e in the animal derived food, a kind of method of implementing be convenient to reliably be provided, can satisfy research and produce in needs.
Embodiment
Embodiment 1, and the precision of polymyxin e residual quantity and the recovery detect in the chicken:
Take by weighing the sample 5.0012g (being accurate to 0.0001g) that pulverized in 50mL tool plug centrifuge tube, add extract 25mL, behind the homogeneous 2min, 4 ℃ of centrifugal 10min down.Shift supernatant to another centrifuge tube, add the 20mL extract in the residue and repeat the above operation of extracting.Merge extract supernatant 2 times after, add normal hexane 20mL vortex 2min, centrifugal 10min discards upper strata liquid.Add normal hexane 20mL in the subnatant again and repeat above degreasing operation, the gained subnatant is to be clean.
Above-mentioned gained sample extract is transferred to Oasis HLB decontaminating column (with each the 6mL prewashing activation of first alcohol and water), uses the 10mL water washing earlier, discard effluent.Use the 3mL methanol-eluted fractions again, collect eluent, nitrogen flows down organic phase is dried up in 40 ℃ of water-baths.Behind 1.00mL, through 0.22 μ m membrane filtration, measure for UPLC-MS/MS by mixing with dissolve with methanol and constant volume for sample.
Take by weighing polymyxin e standard items (purity 97.5%) 10.00mg, with dissolve with methanol and be settled to 10.00mL, concentration is the storing solution of 1.00mg/mL, further uses liquid with 100 times of methyl alcohol dilutions as standard then, and dilution is 0.1,0.2 again, the standard of 0.5ug/mL uses liquid.
Detecting instrument is existing waters Ultra Performance Liquid Chromatography-tandem mass spectrometer:
Liquid phase chromatogram condition
Analytical column: Acquity BEH-C18,2.1mm * 50mm, 1.7 μ m
Moving phase: acetonitrile+0.1% aqueous formic acid=20+80
Flow velocity: 0.2mL/min.
Sample size: 10 μ L.
The mass spectrum condition
Ion gun: electric spray ion source;
Scan mode: positive ion scanning;
Detection mode: multiple-reaction monitoring;
Electron spray voltage: 3.0kv;
Ion source temperature: 110 ℃;
The temperature of desolvating: 400 ℃;
Ion pair, taper hole voltage, collision energy see Table 1.
The ion pair of table 1 polymyxin e, taper hole voltage, collision energy
Qualitative according to retention time, the external standard peak area method is quantitative.
Result of calculation, the computing formula of polymyxin e is in the sample:
In the formula:
The residual quantity of polymyxin e in the X-sample, unit is every kilogram of microgram (ug/kg);
The concentration of polymyxin e (ng/mL) in the C-sample treatment solution;
The final constant volume of V-sample extract, unit are milliliter (ml);
The sample weighting amount of m-sample, unit is gram (g);
In the sample content of polymyxin e by formula (1) calculate, the result is as follows:
Embodiment 2, the detection of the polymyxin e precision and the recovery in the pork liver:
Take by weighing the sample 5.0210g (being accurate to 0.0001g) that pulverized in 50mL tool plug centrifuge tube, add extract 25mL, behind the homogeneous 2min, 4 ℃ of centrifugal 10min down.Shift supernatant to another centrifuge tube, add the 20mL extract in the residue and repeat the above operation of extracting.Merge extract supernatant 2 times after, add normal hexane 20mL vortex 2min, centrifugal 10min discards upper strata liquid.Add normal hexane 20mL in the subnatant again and repeat above degreasing operation, the gained subnatant is waited until purification.
Above-mentioned gained sample extract is transferred to Oasis HLB decontaminating column (with each the 6mL prewashing activation of first alcohol and water), uses the 10mL water washing earlier, discard effluent.Use the 3mL methanol-eluted fractions again, collect eluent, nitrogen flows down organic phase is dried up in 40 ℃ of water-baths.Behind 1.00mL, through 0.22 μ m membrane filtration, measure for UPLC-MS/MS by mixing with dissolve with methanol and constant volume for sample.
Take by weighing polymyxin e standard items (purity 97.5%) 10.00mg, with dissolve with methanol and be settled to 10.00mL, concentration is the storing solution of 1.00mg/mL, further uses liquid with 100 times of methyl alcohol dilutions as standard then, and dilution is 0.1,0.2 again, the standard of 0.5ug/mL uses liquid.
Detecting instrument is existing waters Ultra Performance Liquid Chromatography-tandem mass spectrometer:
Liquid phase chromatogram condition
Analytical column: Acquity BEH-C18,2.1mm * 50mm, 1.7 μ m
Moving phase: acetonitrile+0.1% aqueous formic acid=20+80
Flow velocity: 0.2mL/min.
Sample size: 10 μ L.
The mass spectrum condition
Ion gun: electric spray ion source;
Scan mode: positive ion scanning;
Detection mode: multiple-reaction monitoring;
Electron spray voltage: 3.0kv;
Ion source temperature: 110 ℃;
The temperature of desolvating: 400 ℃;
Ion pair, taper hole voltage, collision energy see Table 1.
The ion pair of table 1 colistin, taper hole voltage, collision energy
Qualitative according to its mass spectra peak, external standard method is quantitative.
Result of calculation, the computing formula of polymyxin e is in the sample:
In the formula:
The residual quantity of polymyxin e in the X-sample, unit is every kilogram of microgram (ug/kg);
The concentration of polymyxin e (ng/mL) in the C-sample treatment solution;
The final constant volume of V-sample extract, unit are milliliter (ml);
The sample weighting amount of m-sample, unit is gram (g);
In the sample residual quantity of polymyxin e by formula (1) calculate, the result is as follows:
Obviously, those of ordinary skill in the art can measure polymyxin e residual quantity in the animal derived food by Ultra Performance Liquid Chromatography-tandem mass spectrometer with a kind of of invention.
The foregoing description is only for the usefulness that the present invention is described; and be not to be limitation of the present invention; the those of ordinary skill in relevant technologies field; without departing from the present invention; can also make various variations and modification; therefore all technical schemes that are equal to also should belong to category of the present invention, and scope of patent protection of the present invention should be limited by each claim.
Claims (7)
1. a superelevation liquid chromatography-tandem mass spectrometry is to the assay method of polymyxin e residual quantity in the animal derived food, and it is characterized in that: described assay method comprises the steps:
Take by weighing the sample 5.0g (being accurate to 0.0001g) that pulverized in 50mL tool plug centrifuge tube, add extract 25mL, behind the homogeneous 2min, 4 ℃ of centrifugal 10min of following 10000r/min.Shift supernatant to another centrifuge tube, add the 20mL extract in the residue and repeat the above operation of extracting.Merge extract supernatant 2 times after, add normal hexane 20mL vortex 2min, the centrifugal 10min of 10000r/min discards upper strata liquid.Add normal hexane 20mL in the subnatant again and repeat above degreasing operation, the gained subnatant is to be clean.
Above-mentioned gained sample extract is transferred to Oasis HLB decontaminating column (with each the 6mL prewashing activation of first alcohol and water), uses the 10mL water washing earlier, discard effluent.Use the 3mL methanol-eluted fractions again, collect eluent, nitrogen flows down organic phase is dried up in 40 ℃ of water-baths.Behind 1.00mL, mixing through 0.22 μ m membrane filtration, obtains sample treatment solution to sample with dissolve with methanol and constant volume.
Take by weighing the polymyxin e standard items, with behind the dissolve with methanol as storing solution, further use liquid for standard then with concentration gradient with methyl alcohol dilution;
Utilize Ultra Performance Liquid Chromatography-series connection level Four bar LC-MS instrument that titer and sample treatment solution are detected;
Result of calculation, the computing formula of polymyxin e is in the sample:
In the formula:
The residual quantity of polymyxin e in the X-sample, unit is every kilogram of microgram (ug/kg);
The concentration of polymyxin e (ng/mL) in the C-sample treatment solution;
The final constant volume of V-sample extract, unit are milliliter (m1);
The sample weighting amount of m-sample, unit is gram (g);
2. a kind of superelevation liquid chromatography-tandem mass spectrometry according to claim 1 is to the assay method of polymyxin e residual quantity in the animal derived food, it is characterized in that: described methyl alcohol and aqueous formic acid (6+4) extract, desirable extract proportioning, better controlled the interference of impurity, and guaranteed the recovery.
3. a kind of superelevation liquid chromatography-tandem mass spectrometry according to claim 1 is characterized in that the assay method of polymyxin e residual quantity in the animal derived food: homogeneous extraction time is 2min, has best mixing extraction efficiency under this condition.
4. a kind of superelevation liquid chromatography-tandem mass spectrometry according to claim 1 is characterized in that the assay method of polymyxin e residual quantity in the animal derived food: centrifugal 10min under 4 ℃ has good separating effect.
5. a kind of superelevation liquid chromatography-tandem mass spectrometry according to claim 1 is characterized in that the assay method of polymyxin e residual quantity in the animal derived food: adopt HLB Solid-Phase Extraction column purification, have good clean-up effect.
6. a kind of superelevation liquid chromatography-tandem mass spectrometry according to claim 1 is characterized in that the assay method of polymyxin e residual quantity in the animal derived food: the described Ultra Performance Liquid Chromatography-tandem mass spectrometer that utilizes to the condition that sample treatment solution detects is:
Liquid phase chromatogram condition
Analytical column: Acquity BEH-C18,2.1mm * 50mm, 1.7 μ m
Moving phase: acetonitrile+0.1% aqueous formic acid=20+80
Flow velocity: 0.2mL/min
Sample size: 10 μ L
The mass spectrum condition
Ion gun: electric spray ion source;
Scan mode: positive ion scanning;
Detection mode: multiple-reaction monitoring;
Electron spray voltage: 3.0kv;
Ion source temperature: 110 ℃;
The temperature of desolvating: 400 ℃;
Ion pair, taper hole voltage, collision energy see Table 1.
The ion pair of table 1 colistin, taper hole voltage, collision energy
Has good separating effect under this condition
7. a kind of superelevation liquid chromatography-tandem mass spectrometry according to claim 1 is characterized in that the assay method of polymyxin e residual quantity in the animal derived food: utilize comparatively advanced, highly sensitive Ultra Performance Liquid Chromatography-tandem mass spectrometer that the residual quantity of polymyxin e in the animal derived food is detected.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104458988A (en) * | 2014-11-27 | 2015-03-25 | 山东出入境检验检疫局检验检疫技术中心 | Method for testing group of biomarkers |
| CN106896172A (en) * | 2017-01-19 | 2017-06-27 | 烟台出入境检验检疫局检验检疫技术中心 | Method for quick being remained a kind of animal derived food herbal medicine more |
| CN108226361A (en) * | 2016-12-15 | 2018-06-29 | 上海医药工业研究院 | A kind of method for analyzing polymyxin E methanesulfonic sodium components |
| CN108226315A (en) * | 2016-12-15 | 2018-06-29 | 上海医药工业研究院 | A kind of analysis method for detecting polymyxin E residual quantities |
| CN110174469A (en) * | 2019-04-24 | 2019-08-27 | 山东省海洋资源与环境研究院 | The detection method of tri- kinds of diarrhetic shellfish poisons of OA, DTX1 and DTX2 in seaweed |
| CN111830153A (en) * | 2020-07-14 | 2020-10-27 | 南京品生医学检验实验室有限公司 | Method for detecting concentrations of polymyxin B1and polymyxin B2 in serum |
| CN114791470A (en) * | 2022-06-24 | 2022-07-26 | 北京和合医学诊断技术股份有限公司 | Method for detecting polymyxin in blood by high performance liquid chromatography-tandem mass spectrometry and application |
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2011
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104458988A (en) * | 2014-11-27 | 2015-03-25 | 山东出入境检验检疫局检验检疫技术中心 | Method for testing group of biomarkers |
| CN104458988B (en) * | 2014-11-27 | 2016-01-20 | 山东出入境检验检疫局检验检疫技术中心 | The assay method of one group of biomarker |
| CN108226361A (en) * | 2016-12-15 | 2018-06-29 | 上海医药工业研究院 | A kind of method for analyzing polymyxin E methanesulfonic sodium components |
| CN108226315A (en) * | 2016-12-15 | 2018-06-29 | 上海医药工业研究院 | A kind of analysis method for detecting polymyxin E residual quantities |
| CN108226361B (en) * | 2016-12-15 | 2021-09-28 | 上海医药工业研究院 | Method for analyzing polymyxin E sodium methanesulfonate component |
| CN108226315B (en) * | 2016-12-15 | 2022-04-12 | 上海医药工业研究院 | Analysis method for detecting polymyxin E residual quantity |
| CN106896172A (en) * | 2017-01-19 | 2017-06-27 | 烟台出入境检验检疫局检验检疫技术中心 | Method for quick being remained a kind of animal derived food herbal medicine more |
| CN110174469A (en) * | 2019-04-24 | 2019-08-27 | 山东省海洋资源与环境研究院 | The detection method of tri- kinds of diarrhetic shellfish poisons of OA, DTX1 and DTX2 in seaweed |
| CN111830153A (en) * | 2020-07-14 | 2020-10-27 | 南京品生医学检验实验室有限公司 | Method for detecting concentrations of polymyxin B1and polymyxin B2 in serum |
| CN114791470A (en) * | 2022-06-24 | 2022-07-26 | 北京和合医学诊断技术股份有限公司 | Method for detecting polymyxin in blood by high performance liquid chromatography-tandem mass spectrometry and application |
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Application publication date: 20111102 |