CN101986153A - Method for determining galaxolide in trace amount in water sample - Google Patents
Method for determining galaxolide in trace amount in water sample Download PDFInfo
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- CN101986153A CN101986153A CN 201010289040 CN201010289040A CN101986153A CN 101986153 A CN101986153 A CN 101986153A CN 201010289040 CN201010289040 CN 201010289040 CN 201010289040 A CN201010289040 A CN 201010289040A CN 101986153 A CN101986153 A CN 101986153A
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Abstract
The invention relates to a method for determining galaxolide in trace amount in water sample by means of the co-utilization of solid phase microextraction (SPME) and GC-MS, belonging to the field of environmental monitoring. The method comprises two steps, namely drawing of a standard curve and determination of samples. The determination of samples is characterized in that water samples are subjected to the filtration of filter membrane (0.45mum), a fixed amount of samples are then put in an extraction flask and subjected to immersed extraction for 40 minutes at 35 DEG C, followed by the analysis of GC-MS intermediately, and finally, the amount is determined by external standard method according to peak appearance area. The method has excellent linearity in the range from 200 to 1500ng/L and 7.9% of RSD according to parallel determination of standard solution. The method also has the advantage of being convenient, fast, accurate and the like, and is particularly suitable for the determination of galaxolide in municipal sewage.
Description
Technical field
The present invention relates to the assay method of trace Jiale muskiness in a kind of water sample, belong to the environmental monitoring field.
Background technology
The synthetic Moschus has been widely used in the daily-use chemical industry industry, and polycyclic musk is wherein just replacing other Moschus, becomes a most widely used class musk ambrette.As the representative of polycyclic musk class material, and Jiale muskiness (1,3,4,6,7,8-hexahydro-4,6,6,7,8,8-hexamethyl-γ-2-chromene, C
18H
26O is called for short HHCB) be widely used in cosmetics, perfume, washing agent, perfumed soap, shampoo, freshener etc., be a kind of purposes polycyclic musk the most widely.For example, the use amount of European Jiale muskiness in 2000 accounts for more than 90% of polycyclic musk total amount.
The cosmetics of everyday use that contains Jiale muskiness is used back discharging water body, accumulates in environment, because its degradable performance is relatively poor, is listed in one of persistent pollutant, and its environmental effect causes more concern.Therefore but compare with other polluter, the assay method of Jiale muskiness does not also have the unified method standard at present in the water body, develops that the Jiale muskiness analytical approach is very important in the feasible water body.
Jiale muskiness in the water body is measured and is related to sample pre-treatments and two steps of sample analysis.Sample-pretreating method is more, and commonly used have liquid-liquid extraction, a Solid-Phase Extraction (SPE) etc., after pre-treatment, carries out gas chromatography, liquid chromatography, gas-analyses such as matter coupling again.Wherein, liquid-liquid extraction method need consume a large amount of toxic organic solvent, be detrimental to health, and contaminated environment, reappearance is relatively poor.Solid-phase extraction device is simple, and solvent-oil ratio is few, but need extract, operations such as drying, wash-out, purging, enrichment, constant volume, length consuming time, complex operation.Solid-phase microextraction (SPME) is the sample pre-treatments technology by the Canadian Waterloo Arhturhe of university and professor's Pawliszyn initiative, treasury is got, is concentrated, desorb, sample introduction be in one, have selectivity height, advantage such as quick easy to use, safe, in gaseous state, water body, the analysis of volatile organic matter, semi-volatile organic matter, inorganics in solid-state, be used widely.But, different target analytes, SPME technical operation parameter is different (as the salinity of the kind of extracting head, analytic sample, pH, extraction mode, time, temperature etc.), need optimize accordingly.
Content of the present invention is at the Jiale muskiness in the water sample, develops a cover SPME-GC-MS method of operating, enables to be applicable to the mensuration of Jiale muskiness in the municipal effluent.
Summary of the invention
The object of the present invention is to provide a kind of SPME-GC-MS of utilization to measure trace Jiale muskiness method in the water sample.
Technical scheme of the present invention:
The assay method of trace Jiale muskiness comprises the steps: in a kind of water sample
(1), standard curve making
A. standard solution preparation:
Accurately take by weighing the Jiale muskiness standard model, at first be dissolved in acetone (analyzing pure), be mixed with 100 μ g/L standard stock solutions; Pipette the series standard stock solution respectively,, obtain the series standard solution of concentration 200～1500ng/L with the pure water dilution;
The b.SPME operation:
Adopt 100 μ mPDMS extracting head, get the standard solution sample that step a prepared of 5～10mL, immerse extraction, 35 ℃ of extraction temperature, extraction time 40min is after extraction is finished, sample introduction immediately, 250 ℃ of GC desorption temperatures enter the GC-MS analytic system behind the desorption time 5min;
C.GC-MS analyzes:
Chromatographic column HP-5 quartz column (30m * 0.25mm * 0.25um); Heating schedule is 80 ℃, rises to 295 ℃ with 10 ℃/min speed, keeps 10min; Carrier gas is a high pure nitrogen, pressure 130.5kPa, flow 1.70mL/min; Split ratio 1:2; 250 ℃ of injector temperatures, 300 ℃ of FID detected temperatures; EI bombards the source, 180 ℃ of ion source temperatures, and SIM scans, and draws the typical curve of Jiale muskiness concentration in peak area and the titer;
(2), sample detection
Water sample through the 0.45um filtering with microporous membrane, is got water sample after the filter of 5～10mL, b.SPME operation and c.GC-MS analysis operation in the repeating step (1), the peak area reference standard curve that draws can be learnt the content of Jiale muskiness in the sample.
Above-mentioned employing acetone preparation standard stock solution is very important, and any ratio of acetone and water characteristic of dissolving each other can guarantee that Jiale muskiness evenly distributes in water, thereby has guaranteed the consistance of SPME extraction efficiency between the different samples.
During SPME extraction Jiale muskiness sample, need not carry out pH and salinity adjustment, our test is bright, and pH and salinity adjustment obviously do not help percentage extraction, even some loss.When sample detection, need in advance water sample to be carried out filtering with microporous membrane, to remove suspended particle wherein, the solid phase adsorption Jiale muskiness is to the interference of test result in the elimination water sample.
The assay method of trace Jiale muskiness in the water sample of the present invention can be applicable to the mensuration of municipal effluent Jiale muskiness.
Technique effect of the present invention
A cover of the present invention utilizes the method for trace Jiale muskiness in SPME-GC-MS fast measuring water sample, and measurement range is 200-1500ng/L, and is consuming time within an hour.The trace Jiale muskiness does not have standard method in the water sample at present, situation from bibliographical information, adopt SPE-GC-MS technical measurement scope suitable, but have SPE (water sample needs 3 hours even more of a specified duration) consuming time, flow process complexity, reappear shortcomings such as rate variance with the present invention.
Description of drawings
Fig. 1, Jiale muskiness mass spectrogram
Fig. 2, Jiale muskiness standard mass spectrogram
Jiale muskiness chromatogram in Fig. 3, the municipal effluent
The canonical plotting of Jiale muskiness concentration in Fig. 4, peak area and the standard solution.Ordinate is a peak area among the figure, and abscissa is concentration of standard solution/ng/L.
Embodiment
Also in conjunction with the accompanying drawings the present invention is further set forth below by embodiment, but do not limit the present invention.
Medicine: Jiale muskiness standard model (10ng/ μ L, 1ml, Shanghai lark waffle learn a skill company limited), acetone (analyze pure, Shanghai traditional Chinese medicines group)
Acetone: analyze pure
Equipment: SPME automatic sampler (Sigma-Aldrich Co.); 100 μ mPDMS extracting head (Sigma-Aldrich Co.); 20ml extraction flask (Sigma-Aldrich Co.); Chromaticness is online: Agilent GC-MS-7890, chromatographic column HP-5 quartz column (30m * 0.25mm * 0.25um), fid detector.
Embodiment 1
The mensuration of Jiale muskiness in the municipal effluent
Standard solution preparation: get the Jiale muskiness standard model, be dissolved in acetone (analyzing pure), being mixed with 100ml concentration is 100 μ g/L standard stock solutions, pipette 0.2 m L, 0.4m L, 0.6mL, 0.8mL, 1mL, 1.2 mL, 1.4mL more respectively, be diluted to 100mL with deionized water, can obtain 200,400,600,800,1000,1200 like this, the series standard solution of 1400ng/L.
The SPME operation: adopt 100 μ mPDMS extracting head, extraction sample size 5g immerses extraction, 35 ℃ of extraction temperature, extraction time 40min.250 ℃ of GC desorption temperatures, desorption time 5min.
GC-MS analyzes: heating schedule is 80 ℃, rises to 295 ℃ with 10 ℃/min speed, keeps 10min.Carrier gas is a high pure nitrogen, pressure 130.5kPa, flow 1.70mL/min; Split ratio 1:2.250 ℃ of injector temperatures, 300 ℃ of FID detected temperatures.EI bombards the source, and 180 ℃ of ion source temperatures are selected ion (SIM) scanning.
With above-mentioned analytic process, the typical curve that draws Jiale muskiness concentration in peak area and the standard solution is Y=458.16X+548006, R
2=0.9958, see Fig. 4.
Get Longhua, Shanghai Sewage Plant water inlet 50ml, water sample is got filter back water sample 5g through the 0.45um filtering with microporous membrane, carries out above-mentioned SPME operation and analyzes with GC-MS, with peak area reference standard curve, can learn that the Jiale muskiness in the Sewage Plant water inlet of Longhua, Shanghai is 286ng/L.
Accompanying drawing 1 Jiale muskiness standard model mass spectrogram, accompanying drawing 2 is the standard mass spectrogram in the instrument mass spectrum picture library, accompanying drawing 3 is intake behind SPME for Sewage Plant, carries out the spectrogram that SIM scanning draws.Can the standard model mass spectrogram from the contrast of accompanying drawing 1 and accompanying drawing 2 and standard mass spectrogram matching rate reach 96%.
Above said content only is the basic explanation of the present invention under conceiving, and according to any equivalent transformation that technical scheme of the present invention is done, all should belong to protection scope of the present invention.
Claims (3)
1. the assay method of trace Jiale muskiness in the water sample is characterized in that comprising the steps:
(1), standard curve making
A. standard solution preparation:
Accurately take by weighing the Jiale muskiness standard model, at first be dissolved in acetone (analyzing pure), be mixed with 100 μ g/L standard stock solutions; Pipette the series standard stock solution respectively,, obtain the series standard solution of concentration 200～1500ng/L with the pure water dilution;
The b.SPME operation:
Adopt 100 μ mPDMS extracting head, get the standard solution sample that step a prepared of 5～10mL, immerse extraction, 35 ℃ of extraction temperature, extraction time 40min is after extraction is finished, sample introduction immediately, 250 ℃ of GC desorption temperatures enter the GC-MS analytic system behind the desorption time 5min;
C.GC-MS analyzes:
Chromatographic column HP-5 quartz column (30m * 0.25mm * 0.25um); Heating schedule is 80 ℃, rises to 295 ℃ with 10 ℃/min speed, keeps 10min, and carrier gas is a high pure nitrogen, pressure 130.5kPa, flow 1.70mL/min; Split ratio 1:2; 250 ℃ of injector temperatures, 300 ℃ of FID detected temperatures; EI bombards the source, 180 ℃ of ion source temperatures, and SIM scans, and draws the typical curve of Jiale muskiness concentration in peak area and the titer;
(2), sample detection
Water sample through the 0.45um filtering with microporous membrane, is got water sample after the filter of 5-10mL, the b.SPME operation of repeating step (1) and c.GC-MS analysis, the peak area reference standard curve that draws can be learnt the content of Jiale muskiness in the sample.
2. the assay method of trace Jiale muskiness is particularly useful for the mensuration of Jiale muskiness in the municipal effluent in a kind of water sample as claimed in claim 1.
3. the assay method of trace Jiale muskiness in a kind of water sample as claimed in claim 1, the detection level scope that it is characterized in that Jiale muskiness is 200～1500ng/L.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102914597A (en) * | 2011-08-02 | 2013-02-06 | 漳州片仔癀药业股份有限公司 | Quality testing method for fingerprint of herbal medicine musk |
| WO2023284346A1 (en) * | 2021-07-15 | 2023-01-19 | 长视科技股份有限公司 | Method for detecting polycyclic musks in water body |
-
2010
- 2010-09-21 CN CN 201010289040 patent/CN101986153A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| 《中国科学院研究生院博士学位论文》 20051231 曾祥英 污水处理厂多环麝香污染物的分布特征及去除途径的初步研究 第27-39页 1-3 , * |
| 《环境监测管理与技术》 20060630 曾祥英等 环境中合成麝香污染物的研究进展 第7-10页 1-3 第18卷, 第3期 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102914597A (en) * | 2011-08-02 | 2013-02-06 | 漳州片仔癀药业股份有限公司 | Quality testing method for fingerprint of herbal medicine musk |
| CN102914597B (en) * | 2011-08-02 | 2014-10-15 | 漳州片仔癀药业股份有限公司 | Quality testing method for fingerprint of herbal medicine musk |
| WO2023284346A1 (en) * | 2021-07-15 | 2023-01-19 | 长视科技股份有限公司 | Method for detecting polycyclic musks in water body |
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Application publication date: 20110316 |