CN103323550A - Method for simultaneously detecting five medicaments in water - Google Patents
Method for simultaneously detecting five medicaments in water Download PDFInfo
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Abstract
The invention discloses a method for simultaneously detecting the medicaments such as furazolidone, diazepam, trimethoprim, acetaminophen and ibuprofen in water. The method comprises the following steps of: filtering a water sample to remove suspended matter; adjusting the pH of the water sample to be 2 to 4; activating hydrophile-lipophile balance (HLB) solid phase extraction column by using acetone, methanol, ammonium acetate-containing formic acid aqueous solution and ultrapure water in sequence; after the enrichment is finished, drying the HLB solid phase extraction column under the protection of nitrogen and eluting the HLB solid phase extraction column; collecting eluant, and drying the eluant by blowing a nitrogen flow; adding acetonitrile to dissolve the residue; and quantitatively detecting the concentration of the five medicaments. By the method, the water sample pretreatment is environment-friendly, easy to operate, large in enrichment factor, and high in reproducibility; and the content of the five common medicaments in a water environment can be analyzed quickly and accurately.
Description
Technical field
The invention belongs to the detection technique field of water environment pollution thing, the detection method that relates to five kinds of common medicines of trace in a kind of water body particularly relates more specifically to a kind of detection method at trace furazolidone, diazepam, Trimethoprim, paracetamol, brufen in the surface water (river).
Background technology
Five kinds of common medicines (furazolidone, diazepam, Trimethoprim, paracetamol and brufen) play crucial effects in daily life.Furazolidone has another name called furazolidone, has advantages such as curative effect height, has a broad antifungal spectrum, is used for the control bacteriosis of aquatic livestock in aquaculture.But studies have shown that furazolidone and cylinder metabolism-ure thereof have mutagenesis carcinogenesis and other toxic and side effects.Diazepam is the hypnotic sedative agent of using always clinically, has calmness, hypnosis, antianxiety, central is of flaccid muscles and anticonvulsant action, and diazepam carries out metabolism through the liver effect in vivo, and these metabolic products are discharged with the form of urine.In recent years, taking diazepam poisons, anaesthetizes with diazepam event such as crime and often take place.Trimethoprim is a kind of broad spectrum antibiotic, the Chang Zuowei synergetic effect additive makes an addition in the multiple antibiotic and makes CD, Trimethoprim has wide application prospect to many new infectious diseases, set up the method that detects Trimethoprim medicament contg and blood concentration in time, exactly, for determining on the clinical treatment that rational dosage regimen, minimizing toxic and side effect take place significant.Paracetamol (paracetamol) is a kind of common amide-type analgesic-antipyretic, be widely used in diseases such as cat fever, headache, arthralgia, neuralgia clinically, but paracetamol also has certain toxic and side effect to human body, excessive use can cause hepatonecrosis, in addition digestive system, respiratory system, urinary system etc. is also had certain influence. and it is significant therefore to measure Paracetamol content.Brufen is mainly from waste water and the slop of producing the pharmacy corporation discharging in the environment, the brufen that the people takes has 8.9%-14% to modify without metabolism or to be excreted to the environment brufen with glucosiduronate in conjunction with attitude not volatile, physical property is stable, half life period is longer, be difficult for precipitated thing absorption, less generation chemical degradation, therefore, be considered to " persistence " environmental contaminants, its residual harm and pollution risk are comparatively serious.
These common medicines generally can not be absorbed fully, be utilized, and medicine or its metabolin will enter environment by approach such as urine, defecate.And the existing treatment technology of sewage treatment plant can not or can not effectively be removed it substantially, and result of study shows that the lactam antibiotics content in the environmental water sample is very little, only is ng/L or μ g/L level.Though concentration range is not enough to cause acute to biology or subacute toxicity is imitated at ng/L to the left drug of μ g/L level in the environment, its mix toxicity and the chronic toxicity effect very important.Given this, need set up a kind of economy, fast, sensitive, accurately and the analytical approach that can analyze multiple common medicine simultaneously be necessary.
Summary of the invention
The object of the present invention is to provide a kind of method that detects five kinds of common medicines in the water simultaneously, can carry out enrichment and quantitative measurement to trace medicine in the water environment sample.
For achieving the above object, the method that detects five kinds of medicines in the water simultaneously provided by the invention, its step is as follows:
(1) pre-service of water sample
Water sample removes by filter suspension, and regulating water sample pH is 2-4, successively with acetone, methyl alcohol, the aqueous formic acid that contains ammonium acetate and ultrapure water activation HLB solid-phase extraction column;
(2) enrichment method
After enrichment is finished, with HLB solid-phase extraction column dry back wash-out HLB Solid-Phase Extraction under nitrogen protection, collect eluent and flow down in nitrogen and dry up, add the acetonitrile dissolution residual substance;
(3) quantitatively detect five kinds of drug concentrations;
Described five kinds of medicines are respectively furazolidone, diazepam, Trimethoprim, paracetamol and brufen.
Described detection method, wherein, the water sample filtration is the GF/F filter membrane with 0.47 μ m in the step 1.
Described detection method wherein, is to add hydrochloric acid or sulfuric acid adjusting water sample pH in the step 1.
Described detection method, wherein, aqueous formic acid contains the ammonium acetate of 5mmol/L in the step 2.
Described detection method, wherein, the water sample in the step 2 is crossed post control flow velocity less than 1mL/min.
Described detection method, wherein, the eluent flow rate of wash-out HLB solid-phase extraction column is less than 1.0mL/min in the step 2.
Described detection method, wherein, the eluent in the step 2 is the methanol solution that contains 5% ammoniacal liquor.
Described detection method, wherein, step 3 is to adopt the liquid chromatography-tandem mass spectrometry method to detect five kinds of drug concentrations.
Described detection method wherein, is to adopt 3200QTrap type liquid chromatography-tandem mass spectrometry instrument quantitatively to detect, wherein: chromatographic column ZORBAX Eclipse XDB C
18, 4.6mm * 150mm * 5 μ m;
3200QTrap type liquid chromatography-tandem mass spectrometry instrument mass spectrum condition is:
Ionization mode: ES (+), ion injection electric: 5500V, taper hole voltage: 34V, source temperature: 580 ℃.
The invention has the beneficial effects as follows and adopt the high performance liquid chromatography-tandem mass coupling that five kinds of medicines are carried out quantitative measurement simultaneously, operation is simple, analyzes fast, and a sample only needs about 5min.Selectivity to target compound is strong, and is quantitatively accurately, highly sensitive.Especially provide a kind of environmental friendliness, easy operating, enrichment multiple height, favorable reproducibility, can be fast the method for multiple medicine in the analyzing water body simultaneously.
Description of drawings
Fig. 1 is the ion flow graph of five kinds of common medicine hybrid standard product solution of 100ng/mL of the present invention, and wherein (a) is the peak sequence of four kinds of ortho-spectrum medicines, is respectively Trimethoprim 3.28min; Paracetamol 3.28min; Furazolidone 4.04min; Diazepam 5.48min.(b) be that negative spectrum brufen mixes mark chromatography of ions figure, brufen 5.03min.
Fig. 2 is the quantitative daughter ion typical curve of furazolidone.
Fig. 3 is the quantitative daughter ion typical curve of diazepam.
Fig. 4 is the quantitative daughter ion typical curve of Trimethoprim.
Fig. 5 is the quantitative daughter ion typical curve of paracetamol.
Fig. 6 is the quantitative daughter ion typical curve of brufen.
Embodiment
The present invention adopts Solid-Phase Extraction-high performance liquid chromatography-tandem mass method to realize trace medicine in the water environment sample is carried out enrichment and quantitative measurement, and operation is simple, analyzes quick and precisely.Can satisfy the requirement that environmental sample detects.
Detection method of the present invention is as follows:
(1) water sample pre-service
River sample 1.0L removes suspension with the GF/F membrane filtration of 0.47 μ m, and adding small amount of hydrochloric acid adjusting water sample pH is about 3.0.(the control flow velocity is less than 1mL/min for 500mg, 6cc) solid-phase extraction column to utilize 6mL chromatographically pure acetone, 6mL chromatographically pure methyl alcohol, 6mL to contain the HLB of 0.1% (m/v) aqueous formic acid, 15-20mL ultrapure water activation Waters company of 5mmol/L ammonium acetate successively;
(2) enrichment method
After enrichment is finished, with HLB solid-phase extraction column dry 20min under nitrogen protection, utilize the ammoniacal liquor methanol solution wash-out HLB post of 10mL5%, the control flow velocity is less than 1mL/min, eluent is collected in the 10mL point end glass centrifuge tube, and eluent flows down slowly to blow until near at nitrogen and does, and adds 400 μ L trifluoroacetic acid aqueous solution dissolution residual substances, whirlpool mixes, and is to be measured;
(3) utilize 3200QTrap type liquid chromatography-tandem mass spectrometry instrument quantitatively to detect five kinds of common medicines
Chromatographic column: ZORBAX Eclipse XDB C
18, 4.6mm * 150mm * 5 μ m;
3200QTrap type liquid chromatography-tandem mass spectrometry instrument mass spectrum condition is as follows:
Ionization mode: ES (+) (brufen is negative spectrum), ion injection electric: 5500V, taper hole voltage: 34V, source temperature: 580 ℃.
With this understanding, five kinds of content of medicines of quantitative measurment.
(4) drawing standard curve carries out quantitative measurement with external standard method
The drafting of described external standard method typical curve: use acetonitrile with an amount of furazolidone of the accurate weighing of analytical balance, diazepam, Trimethoprim, paracetamol, brufen standard items (Dr.E): (v: v) dissolve standard items, be mixed with concentration is single mark stock solution of 1mg/mL to water=1: 1.With pure acetonitrile storing solution is diluted to the mixed standard solution of series concentration then, is transferred in the sample introduction bottle, measure with efficient liquid phase-tandem mass spectrum by above-mentioned condition.Be horizontal ordinate with concentration, response is that ordinate returns, and obtains typical curve, is used for the amount of working sample analyte.
(5) mensuration of sample and the recovery are calculated
Gather water sample to be measured, 1 and 2 pair of water sample carries out pre-service and enrichment method set by step, 3 carries out liquid chromatography-tandem mass spectrometry and detects set by step again, and bring in the typical curve equation of step 4, finally obtains 5 kinds of common drug concentrations in the water sample to be measured by calculating.Utilize the following formula calculate recovery rate:
The R-recovery, %;
C
2The drug concentrations of-interpolation standard solution water sample, μ g/L;
C
1-do not add standard solution water sample drug concentrations, μ g/L;
C
sThe concentration of-adding standard solution, μ g/L;
V
2The volume of-interpolation standard solution water sample, L;
V
1-do not add standard solution water sample, L;
V
sThe volume of-interpolation standard solution, L.
Illustrated below in conjunction with most preferred embodiment and the accompanying drawing detection method to five kinds of common drug concentrations in the water environment of the present invention.
Embodiment 1: recovery experimental result
Get the 1000ml ultrapure water in Brown Glass Brown glass bottles and jars only, every bottle of water sample adds the common medicine hybrid standard of 1ml100 μ g/L5 kind storing solution, and adding small amount of hydrochloric acid adjusting water sample pH behind the mixing is about 3.0.(the control flow velocity is less than 1mL/min for 500mg, 6cc) solid-phase extraction column to utilize 6mL chromatographically pure acetone, 6mL chromatographically pure methyl alcohol, 6mL to contain the HLB of 0.1% (m/v) aqueous formic acid, 15-20mL ultrapure water activation Waters company of 5mmol/L ammonium acetate successively;
(2) enrichment method
After enrichment is finished, with HLB solid-phase extraction column dry 20min under nitrogen protection, utilize the ammoniacal liquor methanol solution wash-out HLB post of 10mL5%, the control flow velocity is less than 1mL/min, eluent is collected in the 10mL point end glass centrifuge tube, and eluent flows down slowly to blow until near at nitrogen and does, and adds 400 μ L trifluoroacetic acid aqueous solution dissolution residual substances, whirlpool mixes, and is to be measured;
(3) utilize 3200QTrap type liquid chromatography-tandem mass spectrometry instrument quantitatively to detect five kinds of common medicines
Chromatographic column: ZORBAX Eclipse XDB C
18, 4.6mm * 150mm * 5 μ m;
3200QTrap type liquid chromatography-tandem mass spectrometry instrument mass spectrum condition is as follows:
Ionization mode: ES (+) (brufen is negative spectrum), ion injection electric: 5500V, taper hole voltage: 34V, source temperature: 580 ℃, with this understanding, five kinds of content of medicines of quantitative measurment.Fig. 1 is the ion flow graph of the common medicine hybrid standard product of five kinds of present embodiment solution, and wherein (a) is the peak sequence of four kinds of ortho-spectrum medicines, is respectively Trimethoprim 3.28min; Paracetamol 3.28min; Furazolidone 4.04min; Diazepam 5.48min.(b) be that negative spectrum brufen mixes mark chromatography of ions figure, brufen 5.03min.
The drafting of external standard method typical curve: five kinds of common medicine mixed standard solutions that storing solution are diluted to 10 μ g/L, 20 μ g/L, 50 μ g/L, 100 μ g/L, 200 μ g/L, 500 μ g/L series concentration with pure acetonitrile, be transferred in the sample introduction bottle, measure with efficient liquid phase-tandem mass spectrum.Be horizontal ordinate with concentration, response is that ordinate returns, and obtains typical curve.Fig. 2 is the quantitative daughter ion typical curve of furazolidone, Fig. 3 is the quantitative daughter ion typical curve of diazepam, Fig. 4 is the quantitative daughter ion typical curve of Trimethoprim, and Fig. 5 is the quantitative daughter ion typical curve of paracetamol, and Fig. 6 is the quantitative daughter ion typical curve of brufen.
Mark-on ultrapure water result is brought in the typical curve equation, finally obtain 5 kinds of common drug concentrations in the water sample to be measured by calculating.Calculate recovery rate, result such as table 1.
Embodiment 2: Beijing Olympic park water sample mark-on reclaims the result.
Get 1000ml Beijing Olympic park river water sample in Brown Glass Brown glass bottles and jars only, carry out the mark-on experiment according to the method among the embodiment 1, get not mark-on of 1000ml river water sample simultaneously, as blank.
The result of water sample behind the mark-on is brought in the typical curve equation, finally obtain 5 kinds of common drug concentrations in the water sample to be measured by calculating.Calculate recovery rate, result such as table 2.
Embodiment 3: Shijiazhuang, Hebei vast sea ditch actual water sample measurement result.
The water sample of 1000mL Ziyahe River vast sea ditch (38 ° of 18 ' 28 " N; 114 ° 24 ' 45 " E), through glass fiber filter (Whatman, 0.45 μ m) carry out negative pressure leaching, filtrate is controlled flow velocity at 2～5mL/min through prior 0.1% (m/v) aqueous formic acid, the 15-20mL ultrapure water activation HLB pillar that contains the 5mmol/L ammonium acetate with 6mL chromatographically pure acetone, 6mL chromatographically pure methyl alcohol, 6mL.Enrichment finishes final vacuum and drains 1min, and the ammoniacal liquor methanol solution wash-out HLB post of 10mL5%, eluent are collected in the 10mL point end glass color comparison tube, eluent flows down slowly to blow until near at nitrogen and does, add 400 μ L trifluoroacetic acid aqueous solution dissolution residual substances, whirlpool mixes, and is to be measured.
Utilize using high performance liquid chromatography tandem mass spectrum to measure five kinds of common drug concentrations in the above-mentioned testing sample.In the result of calculation, furazolidone 3.95ng/L, diazepam does not detect, Trimethoprim 49.20ng/L, paracetamol 1136.00ng/L, brufen 44.80ng/L.
Table 1
Table 2
Claims (9)
1. method that detects five kinds of medicines in the water simultaneously, its step is as follows:
(1) pre-service of water sample
Water sample removes by filter suspension, and regulating water sample pH is 2-4, successively with acetone, methyl alcohol, the aqueous formic acid that contains ammonium acetate and ultrapure water activation HLB solid-phase extraction column;
(2) enrichment method
After enrichment is finished, with HLB solid-phase extraction column dry back wash-out HLB Solid-Phase Extraction under nitrogen protection, collect eluent and flow down in nitrogen and dry up, add the acetonitrile dissolution residual substance;
(3) quantitatively detect five kinds of drug concentrations;
Described five kinds of medicines are respectively furazolidone, diazepam, Trimethoprim, paracetamol and brufen.
2. detection method according to claim 1, wherein, to filter be GF/F filter membrane with 0.47 μ m to water sample in the step 1.
3. detection method according to claim 1 wherein, is to add hydrochloric acid or sulfuric acid adjusting water sample pH in the step 1.
4. detection method according to claim 1, wherein, aqueous formic acid contains the ammonium acetate of 5mmol/L in the step 2.
5. detection method according to claim 1, wherein, the water sample in the step 2 is crossed post control flow velocity less than 1mL/min.
6. detection method according to claim 1, wherein, the eluent flow rate of wash-out HLB solid-phase extraction column is less than 1.0mL/min in the step 2.
7. detection method according to claim 1, wherein, the eluent in the step 2 is the methanol solution that contains volume ratio 5% ammoniacal liquor.
8. detection method according to claim 1, wherein, step 3 is to adopt the liquid chromatography-tandem mass spectrometry method to detect five kinds of drug concentrations.
9. detection method according to claim 8 wherein, is to adopt 3200QTrap type liquid chromatography-tandem mass spectrometry instrument quantitatively to detect, wherein:
Chromatographic column ZORBAX Eclipse XDB C
18, 4.6mm * 150mm * 5 μ m;
3200QTrap type liquid chromatography-tandem mass spectrometry instrument mass spectrum condition is:
Ionization mode: ES (+), ion injection electric: 5500V, taper hole voltage: 34V, source temperature: 580 ℃.
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Cited By (8)
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| CN103616467A (en) * | 2013-11-25 | 2014-03-05 | 广东省中山市质量计量监督检测所 | Method for detecting residual tranquilizer medicines in meat product |
| CN104568562A (en) * | 2014-12-31 | 2015-04-29 | 中国地质大学（武汉） | Water sample and pretreatment method of nitrosoamine compound in suspended matter of water sample |
| CN104678040A (en) * | 2015-02-05 | 2015-06-03 | 中国农业科学院兰州畜牧与兽药研究所 | Method for detecting diaveridine, trimethoprim and methyl diaveridine in feed |
| CN105891366A (en) * | 2016-04-25 | 2016-08-24 | 广西壮族自治区梧州食品药品检验所 | Method for determining effective ingredients in cefalexin and trimethoprim capsules by ASE-HPLC (accelerated solvent extractor and high performance liquid chromatography) |
| CN105954398A (en) * | 2016-04-25 | 2016-09-21 | 广西壮族自治区梧州食品药品检验所 | Method for detecting content of cefalexin and trimethoprim in cefalexin and trimethoprim capsule |
| CN108760952A (en) * | 2018-05-11 | 2018-11-06 | 上海大学 | Method for detecting non-steroidal anti-inflammatory drugs in water |
| CN113267580A (en) * | 2021-05-18 | 2021-08-17 | 中南民族大学 | Method for monitoring diazepam blood concentration |
| WO2022270105A1 (en) * | 2021-06-24 | 2022-12-29 | 株式会社島津製作所 | Virus sample concentrating method |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103616467A (en) * | 2013-11-25 | 2014-03-05 | 广东省中山市质量计量监督检测所 | Method for detecting residual tranquilizer medicines in meat product |
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| CN104568562A (en) * | 2014-12-31 | 2015-04-29 | 中国地质大学（武汉） | Water sample and pretreatment method of nitrosoamine compound in suspended matter of water sample |
| CN104678040A (en) * | 2015-02-05 | 2015-06-03 | 中国农业科学院兰州畜牧与兽药研究所 | Method for detecting diaveridine, trimethoprim and methyl diaveridine in feed |
| CN105891366A (en) * | 2016-04-25 | 2016-08-24 | 广西壮族自治区梧州食品药品检验所 | Method for determining effective ingredients in cefalexin and trimethoprim capsules by ASE-HPLC (accelerated solvent extractor and high performance liquid chromatography) |
| CN105954398A (en) * | 2016-04-25 | 2016-09-21 | 广西壮族自治区梧州食品药品检验所 | Method for detecting content of cefalexin and trimethoprim in cefalexin and trimethoprim capsule |
| CN108760952A (en) * | 2018-05-11 | 2018-11-06 | 上海大学 | Method for detecting non-steroidal anti-inflammatory drugs in water |
| CN113267580A (en) * | 2021-05-18 | 2021-08-17 | 中南民族大学 | Method for monitoring diazepam blood concentration |
| CN113267580B (en) * | 2021-05-18 | 2022-09-20 | 中南民族大学 | Method for monitoring diazepam blood concentration |
| WO2022270105A1 (en) * | 2021-06-24 | 2022-12-29 | 株式会社島津製作所 | Virus sample concentrating method |
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Application publication date: 20130925 |