CN115508475A - Method for detecting content of diphenoxylate in sewage - Google Patents
Method for detecting content of diphenoxylate in sewage Download PDFInfo
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- CN115508475A CN115508475A CN202211355498.4A CN202211355498A CN115508475A CN 115508475 A CN115508475 A CN 115508475A CN 202211355498 A CN202211355498 A CN 202211355498A CN 115508475 A CN115508475 A CN 115508475A
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- diphenoxylate
- sewage
- fiber bag
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- HYPPXZBJBPSRLK-UHFFFAOYSA-N diphenoxylate Chemical compound C1CC(C(=O)OCC)(C=2C=CC=CC=2)CCN1CCC(C#N)(C=1C=CC=CC=1)C1=CC=CC=C1 HYPPXZBJBPSRLK-UHFFFAOYSA-N 0.000 title claims abstract description 112
- 229960004192 diphenoxylate Drugs 0.000 title claims abstract description 112
- 239000010865 sewage Substances 0.000 title claims abstract description 72
- 238000000034 method Methods 0.000 title claims abstract description 39
- 238000001179 sorption measurement Methods 0.000 claims abstract description 70
- 239000002245 particle Substances 0.000 claims abstract description 57
- 239000000835 fiber Substances 0.000 claims abstract description 55
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 14
- 239000012498 ultrapure water Substances 0.000 claims abstract description 14
- 238000005406 washing Methods 0.000 claims abstract description 14
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 11
- 238000007664 blowing Methods 0.000 claims abstract description 8
- 230000008569 process Effects 0.000 claims abstract description 7
- 238000011049 filling Methods 0.000 claims abstract description 6
- 238000002386 leaching Methods 0.000 claims abstract description 5
- 238000002791 soaking Methods 0.000 claims abstract description 4
- 238000005086 pumping Methods 0.000 claims abstract description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 24
- 238000012360 testing method Methods 0.000 claims description 24
- 239000003365 glass fiber Substances 0.000 claims description 16
- 239000003463 adsorbent Substances 0.000 claims description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 239000011347 resin Substances 0.000 claims description 8
- 229920005989 resin Polymers 0.000 claims description 8
- 239000000741 silica gel Substances 0.000 claims description 8
- 229910002027 silica gel Inorganic materials 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 7
- 230000010355 oscillation Effects 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 238000011010 flushing procedure Methods 0.000 claims description 2
- GBMDVOWEEQVZKZ-UHFFFAOYSA-N methanol;hydrate Chemical compound O.OC GBMDVOWEEQVZKZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000012535 impurity Substances 0.000 abstract description 12
- 239000000126 substance Substances 0.000 abstract description 11
- 238000001514 detection method Methods 0.000 abstract description 8
- 238000000622 liquid--liquid extraction Methods 0.000 abstract description 5
- 239000002904 solvent Substances 0.000 abstract description 5
- 238000000638 solvent extraction Methods 0.000 abstract description 5
- 238000004587 chromatography analysis Methods 0.000 abstract description 4
- 239000000945 filler Substances 0.000 abstract description 2
- 239000012086 standard solution Substances 0.000 description 25
- 239000011521 glass Substances 0.000 description 13
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 12
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 12
- 239000012528 membrane Substances 0.000 description 12
- 238000001914 filtration Methods 0.000 description 8
- 239000007864 aqueous solution Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 230000002349 favourable effect Effects 0.000 description 6
- 239000000243 solution Substances 0.000 description 5
- 238000010828 elution Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000003795 desorption Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 230000035699 permeability Effects 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 229940079593 drug Drugs 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 206010012335 Dependence Diseases 0.000 description 1
- 206010013496 Disturbance in attention Diseases 0.000 description 1
- 241000287828 Gallus gallus Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 229920002301 cellulose acetate Polymers 0.000 description 1
- 238000009535 clinical urine test Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000003480 eluent Substances 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- NPUKDXXFDDZOKR-LLVKDONJSA-N etomidate Chemical compound CCOC(=O)C1=CN=CN1[C@H](C)C1=CC=CC=C1 NPUKDXXFDDZOKR-LLVKDONJSA-N 0.000 description 1
- 229960001690 etomidate Drugs 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 231100001231 less toxic Toxicity 0.000 description 1
- 238000004895 liquid chromatography mass spectrometry Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000002414 normal-phase solid-phase extraction Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 210000002700 urine Anatomy 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
- B01D15/14—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the introduction of the feed to the apparatus
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/08—Preparation using an enricher
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/08—Preparation using an enricher
- G01N2030/085—Preparation using an enricher using absorbing precolumn
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a method for detecting the content of diphenoxylate in sewage, which belongs to the field of sewage detection and comprises the following steps: filling a fiber bag with diphenoxylate adsorption capacity with adsorption particles; the adsorption capacity of the fiber bag to the diphenoxylate is below that of the adsorption particles; soaking the fiber bag in sample sewage for more than 1 hour; taking out the fiber bag, and washing all the adsorption particles in the fiber bag into the hollow column tube by using ultrapure water; after leaching, pumping, eluting, nitrogen blowing and redissolving, the machine is tested. According to the method, water-permeable fiber bags are used for wrapping adsorption particles, insoluble substances in sewage are isolated, the adsorption particles can adsorb the diphenoxylate from a slightly clean sewage sample, the adsorption particles adopt a common filler of a chromatographic column, the adsorption particles can be directly filled into an empty column after adsorbing the sewage sample, so that the diphenoxylate can be detected by a chromatography method or a derivative method of the chromatography method in the follow-up process, a liquid-liquid extraction method is not needed, the use amount of a solvent is reduced, and the content of the diphenoxylate in the sewage can be accurately determined by avoiding impurity interference.
Description
Technical Field
The invention relates to a method for detecting the content of diphenoxylate in sewage, belonging to the field of sewage detection.
Background
The diphenoxylate has certain addiction, and the tracking and detection of the diphenoxylate content in the sewage is beneficial to the investigation of people who abuse the drugs. Different from direct urine test, a large amount of impurities exist in sewage, and after urine diffuses in the sewage, the content of diphenoxylate in the sewage is very low, so that the diphenoxylate can not be detected by simple means such as test paper.
When detecting trace substances in sewage, a chromatographic column is usually used, impurities in the sewage are many, a filtering membrane is required to be pre-filtered before passing through the chromatographic column, and the main materials of the filtering membrane are glass fiber and cellulose acetate. When the content of the diphenoxylate in the sewage is detected, the molecular structure of the diphenoxylate can enable the diphenoxylate to be adsorbed by a filtering membrane, the detection result is influenced after adsorption, if the filtering membrane is leached by acetonitrile solution for desorption, a plurality of impurities can be leached at the same time, and the detection of the diphenoxylate is also not facilitated. Therefore, at present, the diphenoxylate in the wastewater is detected, and is extracted by a liquid-liquid extraction method and then passes through a chromatographic column, so that a large amount of solution is wasted, and toxic chloroform is used.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a method for detecting the content of diphenoxylate in sewage, which can detect the diphenoxylate in the sewage by using a chromatography, avoid adopting a liquid-liquid extraction method and reduce the using amount of a solvent.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a method for detecting the content of diphenoxylate in sewage comprises the following steps:
loading adsorption particles into a fiber bag with diphenoxylate adsorption capacity; the adsorption capacity of the fiber bag to the diphenoxylate is below that of the adsorption particles;
soaking the fiber bag in sample sewage for more than 1 hour;
taking out the fiber bag, and washing all the adsorption particles in the fiber bag into an empty column tube by using ultrapure water;
and (4) performing machine test after leaching, draining, eluting, nitrogen blowing and redissolving.
The method for detecting the content of the diphenoxylate in the sewage does not need to utilize a liquid-liquid extraction method, is favorable for reducing the using amount of a solvent, can reduce the interference of impurities in the sewage on detection, and can accurately measure the diphenoxylate in the sewage.
Furthermore, the fiber bag is made of glass fibers; the adsorption particles are obtained by mixing full-porous resin and silica gel adsorbent. The fibre bag is used for wrapping up the adsorption particle, avoid the adsorption particle to scatter in the sewage sample, and be used for on the insoluble substance adhesion of isolated sewage arrived the adsorption particle, consequently the fibre bag need have water permeability and certain diphenoxylate adsorption efficiency, make diphenoxylate can pass the fibre bag and contact with the adsorption particle, and the adsorption particle needs to be stronger than the fibre bag or is equivalent with the fibre bag to diphenoxylate, avoid the fibre bag to rob the diphenoxylate that adsorbs on the adsorption particle.
Further, the mixing ratio by mass of the fully porous resin and the silica gel adsorbent is 2:1, better adsorption effect can be obtained.
Further, the step of flushing all the adsorption particles in the bag into the empty column tube by using ultrapure water comprises the following steps: and (3) washing all the adsorption particles in the bag into an empty column tube by using ultrapure water, turning the inside and the outside of the fiber bag, filling the fiber bag into the same column tube, placing the fiber bag on the adsorption particles, and washing the column tube by using the ultrapure water. Because the fiber bag also has certain ability of adsorbing the diphenoxylate, the fiber bag is also plugged into the column tube, and the fiber bag and the adsorption particles are leached and eluted simultaneously, which is favorable for accurately measuring the diphenoxylate content in the sewage. After the fiber bag is turned inside and outside, insoluble substances in the sewage originally adhered to the surface of the fiber bag are changed to be wrapped by the fiber bag, so that the influence on leaching and elution is reduced, and the subsequent regeneration treatment of the adsorption particles is facilitated.
Further, the step of soaking the fiber bag in the sample sewage for more than 1 hour comprises:
the fiber bag was immersed in sample sewage, shaken for 10 minutes, and then allowed to stand at 4 ℃ for 1 hour, and thus the process of shaking and standing was repeated 3 times. After the absorption, the diphenoxylate that the sewage in the fibre bag contained is adsorbed the adsorption particle, diphenoxylate concentration in this part sewage is less than the outer sewage of bag, it is slower to rely on concentration gradient transfer diphenoxylate alone, it is favorable to renewing the sewage in the fibre bag to vibrate, and be favorable to getting rid of the insoluble substance of adhesion on the fibre bag surface, the adsorption particle continues to adsorb the diphenoxylate in the sewage after the renewal when stewing, so circulate, be favorable to the adsorption particle fully to adsorb the diphenoxylate in the sample. Standing in an environment of 4 ℃, which is favorable for cooling, crystallizing and separating out part of impurities in the sewage and reducing the adsorption of the adsorbent to the impurities.
Further, the step of rinsing comprises: rinsed with 10% acetone solution.
Further, the step of eluting comprises: eluted with 70% methanol solution.
Further, the on-machine test uses a LC-MS.
Further, the step of reconstituting comprises: add 20% methanol water to the nitrogen-blown tube, vortex and shake for 1min.
Further, after the vortex oscillation, the method also comprises the following steps: and centrifuging the redissolved solution. More impurities exist in sewage, although the sewage is protected by a fiber bag, in order to ensure the permeability of the fiber bag, the fiber bag can only isolate insoluble substances with larger sizes (more than 1 mm), and after the step of vortex oscillation, a sample is still turbid sometimes and is subjected to centrifugal treatment, but the sample is not filtered, so that the requirement of on-machine testing is met, the volume of the sample is strictly controlled, and the concentration loss of the diphenoxylate caused by filtering is avoided.
The beneficial effects of the invention are: according to the method for detecting the content of the diphenoxylate in the sewage, disclosed by the invention, the adsorption particles are wrapped by the permeable fiber bags, insoluble substances in the sewage are isolated, so that the adsorption particles can adsorb the diphenoxylate from a slightly clean sewage sample, the adsorption particles adopt the filler which has an adsorption effect on the diphenoxylate and belongs to a common chromatographic column, and the adsorbent particles can be directly filled into a hollow column after adsorbing the sewage sample, so that the diphenoxylate can be detected by a chromatography method or a derivative method thereof in the subsequent process, a liquid-liquid extraction method is not needed, the use amount of a solvent is favorably reduced, and the content of the diphenoxylate in the sewage can be accurately determined by avoiding impurity interference.
Additional features and advantages of the application will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by the practice of the application. The objectives and other advantages of the application may be realized and attained by the structure particularly pointed out in the written description.
Detailed Description
The solid-phase extraction column is filtered by a filter membrane in advance, otherwise, the sewage contains a large amount of impurities and even insoluble substances, and the detection accuracy is seriously influenced. The reason why the filter membrane adsorbs diphenoxylate is related to the molecular structure of diphenoxylate, and other ester drugs do not necessarily have similar problems, for example etomidate is not adsorbed on the pre-filtered filter membrane. After the filtering membrane adsorbs the diphenoxylate, acetonitrile can be used for elution to realize desorption, however, after the acetonitrile is used for elution, not only diphenoxylate but also other impurities are eluted, the function of the filtering membrane cannot be exerted, the filtering membrane only plays a role in blocking insoluble substances, and the accurate detection of the diphenoxylate in the sewage is difficult.
Therefore, the embodiment of the application provides a method for detecting the content of diphenoxylate in sewage, which comprises the following steps:
loading adsorption particles into a fiber bag with diphenoxylate adsorption capacity; the adsorption capacity of the fiber bag to diphenoxylate is below that of the adsorption particles. The fiber bags were soaked in the sample wastewater for more than 1 hour. The fiber bag is taken out, and all the adsorption particles in the bag are washed into the hollow column tube by ultrapure water. After leaching, pumping, eluting, nitrogen blowing and redissolving, the machine is tested.
The fiber bag is used for wrapping the adsorption particles, avoiding the adsorption particles from scattering in a sewage sample, and is used for isolating insoluble substances in the sewage, and avoiding the insoluble substances from adhering to the adsorption particles. In the adsorption process, the diphenoxylate contained in the sewage in the fiber bag is adsorbed to the adsorption particles, the diphenoxylate concentration in the part of the sewage is lower than that in the sewage outside the bag, and the diphenoxylate is reliably transferred in a concentration gradient manner. If the fibrous bag excludes diphenoxylate, diphenoxylate is difficult to pass through the fibrous bag and is adsorbed by the adsorbent particles, which affects the effect of transferring diphenoxylate by means of concentration gradient, therefore, the fibrous bag needs to have water permeability and a certain diphenoxylate adsorption capacity, so that diphenoxylate can pass through the fibrous bag and contact with the adsorbent particles. On the other hand, the adsorption capacity of the fiber bag to the diphenoxylate should not be too strong, and preferably weaker than that of the adsorption particles, so as not to rob the diphenoxylate adsorbed on the adsorption particles by the fiber bag.
Sampling test: 5L of sewage is sampled from the water inlet of the sewage treatment plant, and the test is carried out according to the following examples and comparative examples, wherein the measured pH = 7.
Example 1
Respectively measuring 50mL of sewage into five sample bottles of No. 11, no. 12, no. 13, no. 14 and No. 15, and respectively adding standard solutions into the sample bottles, wherein 50 mu l of standard solution containing 100ng/mL diphenoxylate is added into the No. 11 sample bottle; adding 50 μ l of standard solution containing 200ng/mL diphenoxylate into the sample bottle # 12; adding 50 μ l of standard solution containing 500ng/mL diphenoxylate into the 13# sample bottle; adding 50 μ l of standard solution containing 800ng/mL diphenoxylate into a No. 14 sample bottle; sample bottle # 15 was filled with 50. Mu.l of a standard solution containing 1000ng/mL diphenoxylate. The following operations were performed for each of the five sample bottles.
Weighing 100mg of adsorption particles, putting the adsorption particles into a glass fiber bag, fastening the opening of the bag, putting the glass fiber bag into a sample bottle, oscillating for 10 minutes, standing for 1 hour in an environment at 4 ℃, repeating the oscillation-standing process, and counting three cycles. Wherein the adsorption particles are a mixture of XAD-macroporous resin and silica gel adsorbent, and comprise 10 parts of XAD-macroporous resin and 1 part of silica gel adsorbent by mass. Preparing a 6ml hollow column tube, fishing out the glass fiber bag, completely washing the adsorption particles in the bag to the hollow column tube by using ultrapure water under negative pressure, overturning the glass fiber bag inside and outside, filling the glass fiber bag into the column tube, placing the glass fiber bag on the adsorption particles, washing the sample bottle for 5 times by using the ultrapure water, and completely flowing washing liquid through the column tube. 2ml of 10% acetone was added to rinse the column and the column was drained for 1 hour. A disposable needle is connected to the lower end of the column tube, points to the glass test tube, and is eluted by 2ml of 70% methanol aqueous solution. The glass test tube was placed in a nitrogen-blowing apparatus and blown nearly dry with nitrogen. And (3) adding 0.5ml of 20% methanol aqueous solution into the glass test tube after the nitrogen blowing, carrying out vortex oscillation for 1min, centrifuging the mixture on a centrifugal machine, and finally transferring the mixture to a sample injection bottle for a liquid chromatograph-mass spectrometer for testing.
The concentration of the sample diphenoxylate corresponding to the 11# sample bottle is 99.09ng/L, the concentration of the sample diphenoxylate corresponding to the 12# sample bottle is 198.97ng/L, the concentration of the sample diphenoxylate corresponding to the 13# sample bottle is 499.12ng/L, the concentration of the sample diphenoxylate corresponding to the 14# sample bottle is 798.78ng/L, and the concentration of the sample diphenoxylate corresponding to the 15# sample bottle is 999.03ng/L.
Example 2
Respectively measuring 50mL of sewage into five sample bottles of No. 21, no. 22, no. 23, no. 24 and No. 25, and respectively adding standard solutions into the sample bottles, wherein 50 mu l of standard solution containing 100ng/mL diphenoxylate is added into the No. 21 sample bottle; adding 50 μ l of standard solution containing 200ng/mL diphenoxylate into a sample bottle # 22; adding 50 mu l of standard solution containing 500ng/mL diphenoxylate into a sample bottle No. 23; adding 50 μ l of standard solution containing 800ng/mL diphenoxylate into a No. 24 sample bottle; the 25# sample bottle was filled with 50. Mu.l of a standard solution containing 1000ng/mL diphenoxylate. The following operations were performed for each of the five sample bottles.
Weighing 100mg of adsorption particles, putting the adsorption particles into a glass fiber bag, fastening the opening of the bag, putting the glass fiber bag into a sample bottle, oscillating for 10 minutes, standing for 1 hour in an environment at 4 ℃, repeating the oscillation-standing process, and counting three cycles. Wherein the adsorption particles are a mixture of XAD-macroporous resin and silica gel adsorbent, and comprise 2 parts of XAD-macroporous resin and 1 part of silica gel adsorbent by mass. Preparing a 6ml empty column tube, fishing out a glass fiber bag, completely washing adsorption particles in the bag into the empty column tube by using ultrapure water under negative pressure, overturning the glass fiber bag inside and outside, filling the glass fiber bag into the column tube, placing the glass fiber bag on the adsorption particles, washing a sample bottle for 5 times by using ultrapure water, and allowing washing liquid to completely flow through the column tube. 2ml of 10% acetone was added to rinse the column and the column was drained for 1 hour. A disposable needle is connected to the lower end of the column tube, points to the glass test tube, and is eluted by 2ml of 70% methanol aqueous solution. The glass test tube was placed in a nitrogen blower and blown nearly dry with nitrogen. And (3) adding 0.5ml of 20% methanol aqueous solution into the glass test tube after the nitrogen blowing, carrying out vortex oscillation for 1min, centrifuging the glass test tube on a centrifuge, and finally transferring the glass test tube to a sample injection bottle for liquid chromatograph-mass spectrometer test.
The concentration of the sample diphenoxylate corresponding to the 21# sample bottle is 99.95ng/L, the concentration of the sample diphenoxylate corresponding to the 22# sample bottle is 199.97ng/L, the concentration of the sample diphenoxylate corresponding to the 23# sample bottle is 500.12ng/L, the concentration of the sample diphenoxylate corresponding to the 24# sample bottle is 800.01ng/L, and the concentration of the sample diphenoxylate corresponding to the 25# sample bottle is 1000.10ng/L.
Comparative example 1
Respectively measuring 50mL of sewage into five sample bottles of 31#, 32#, 33#, 34# and 35#, and respectively adding standard solution into the sample bottles, wherein 50 mu l of standard solution containing 100ng/mL diphenoxylate is added into the 31# sample bottle; adding 50 μ l of standard solution containing 200ng/mL diphenoxylate into a 32# sample bottle; adding 50 mu l of standard solution containing 500ng/mL diphenoxylate into a No. 33 sample bottle; 34# sample bottle 50. Mu.l standard solution containing 800ng/mL diphenoxylate was added; the 35# sample bottle was filled with 50. Mu.l of a standard solution containing 1000ng/mL diphenoxylate. The following operations were performed for each of the five sample bottles.
Measuring 50mL of chloroform, pouring the chloroform into a separating funnel, pouring the sample in a sample bottle into the separating funnel, shaking the sample bottle on the separating funnel for 1 hour by a shaker, standing for 10 minutes for layering, discharging the lower layer of chloroform into a chicken heart bottle, evaporating the chloroform to dryness by using a rotary evaporator, redissolving the chloroform by using 0.5mL of 20% methanol aqueous solution, and testing by using a liquid chromatography-mass spectrometer.
The concentration of diphenoxylate of the sample corresponding to the 31# sample bottle is 99.82ng/L, the concentration of diphenoxylate of the sample corresponding to the 32# sample bottle is 199.95ng/L, the concentration of diphenoxylate of the sample corresponding to the 33# sample bottle is 499.69ng/L, the concentration of diphenoxylate of the sample corresponding to the 34# sample bottle is 800.34ng/L, and the concentration of diphenoxylate of the sample corresponding to the 35# sample bottle is 999.97ng/L.
Comparative example 2
Respectively measuring 50mL of sewage into five sample bottles of No. 41, no. 42, no. 43, no. 44 and No. 45, and respectively adding standard solutions into the sample bottles, wherein 50 mu l of standard solution containing 100ng/mL diphenoxylate is added into the No. 41 sample bottle; adding 50 μ l of standard solution containing 200ng/mL diphenoxylate into a 42# sample bottle; adding 50 μ l of standard solution containing 500ng/mL diphenoxylate into a 43# sample bottle; adding 50 μ l of standard solution containing 800ng/mL diphenoxylate into a 44# sample bottle; sample bottle # 45 was filled with 50. Mu.l of a standard solution containing 1000ng/mL diphenoxylate. The following operations were performed for each of the five sample bottles.
50mL of sample is sucked by an injector, then a stainless steel needle tube is pulled out, a glass filter membrane is sleeved at the head end of the injector, a piston is pressed down with force, sewage is filtered by the glass fiber filter membrane, then the piston is pulled out, acetonitrile is directly added into the injector for elution, eluent is collected to a glass test tube through an outlet of the injector, and nitrogen is blown to be nearly dry. And (3) adding 0.5ml of 20% methanol aqueous solution into the glass test tube after nitrogen blowing, carrying out vortex oscillation for 1min, centrifuging the glass test tube on a centrifuge, and finally transferring the glass test tube to a liquid chromatograph on a sample injection bottle for testing.
The concentration of the sample diphenoxylate corresponding to the 41# sample bottle is 95.36 ng/L, the concentration of the sample diphenoxylate corresponding to the 42# sample bottle is 204.23ng/L, the concentration of the sample diphenoxylate corresponding to the 43# sample bottle is 502.85 ng/L, the concentration of the sample diphenoxylate corresponding to the 44# sample bottle is 784.21 ng/L, and the concentration of the sample diphenoxylate corresponding to the 45# sample bottle is 942.15 ng/L.
The result of comparative example 1 was observed, and it was confirmed that the originally collected sewage was a negative sample. Comparing the above test results, it can be seen that the results obtained in examples 1, 2 and 1 are similar, and are consistent with the concentration relationship of the sample added into the standard solution, which is a reliable test method, while the solvents used in examples 1 and 2 are less and less toxic than the comparative example 1, which is beneficial to the health of experimenters, and the results obtained in example 2 are more accurate than the results obtained in example 1. Comparative example 2 was affected by impurities reintroduced by desorption, and the deviation from the true value was large, and the concentration of diphenoxylate in the wastewater could not be accurately measured.
In the description of the present specification, reference to the terms "one embodiment," "certain embodiments," "an illustrative embodiment," "an example," "a specific example," or "some examples" or the like means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.
Claims (10)
1. A method for detecting the content of diphenoxylate in sewage is characterized by comprising the following steps:
filling a fiber bag with diphenoxylate adsorption capacity with adsorption particles; the adsorption capacity of the fiber bag to the diphenoxylate is below that of the adsorption particles;
soaking the fiber bag in sample sewage for more than 1 hour;
taking out the fiber bag, and washing all the adsorption particles in the fiber bag into an empty column tube by using ultrapure water;
after leaching, pumping, eluting, nitrogen blowing and redissolving, the machine is tested.
2. The method for detecting the content of diphenoxylate in sewage according to claim 1, wherein the material of the fiber bag is glass fiber; the adsorption particles are obtained by mixing full-porous resin and silica gel adsorbent.
3. The method for detecting the content of diphenoxylate in sewage according to claim 2, wherein the mixing ratio of the fully porous resin to the silica gel adsorbent is 2:1.
4. the method for detecting the content of diphenoxylate in sewage according to claim 1, wherein the step of flushing all the adsorption particles in the bag into the empty column tube with ultrapure water comprises: and (3) washing all the adsorption particles in the bag into an empty column tube by using ultrapure water, turning the fiber bag inside and outside, filling the fiber bag into the same column tube, placing the fiber bag on the adsorption particles, and washing the column tube by using the ultrapure water.
5. The method according to claim 1, wherein the step of immersing the fiber bag in the sample sewage for 1 hour or more comprises:
the fiber bag was soaked in sample sewage, shaken for 10 minutes, and then allowed to stand at 4 ℃ for 1 hour, and the process of shaking and standing was repeated 3 times in total.
6. The method for detecting the content of diphenoxylate in sewage according to claim 1, wherein the step of washing comprises: rinsing with 10% acetone solution.
7. The method for detecting the content of diphenoxylate in sewage according to claim 1, wherein the step of eluting comprises: eluted with 70% methanol solution.
8. The method for detecting the content of diphenoxylate in sewage according to claim 1, wherein the on-machine test uses a liquid chromatograph-mass spectrometer.
9. The method for detecting the content of diphenoxylate in sewage according to claim 1, wherein the redissolving step comprises: add 20% methanol water to the nitrogen-blown tube and vortex for 1min.
10. The method for detecting the content of diphenoxylate in sewage according to claim 9, wherein after the vortex oscillation, the method further comprises the following steps: and (4) centrifuging the redissolved solution.
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