CN112082832B - Method for preserving sulfate combination and glucuronic acid combination in urban sewage - Google Patents
Method for preserving sulfate combination and glucuronic acid combination in urban sewage Download PDFInfo
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- CN112082832B CN112082832B CN201910504875.8A CN201910504875A CN112082832B CN 112082832 B CN112082832 B CN 112082832B CN 201910504875 A CN201910504875 A CN 201910504875A CN 112082832 B CN112082832 B CN 112082832B
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Abstract
The invention belongs to the field of environment, and discloses a method for preserving sulfate conjugates and glucuronide conjugates in urban sewage. Namely, the pH of the sewage is adjusted to 11-14. The invention realizes the effective preservation of the sulfate conjugate and the glucuronic acid conjugate under the condition of high pH value, has the advantages of convenient operation, low cost, good preservation effect and the like, can be widely applied to the preservation of liquid samples such as sewage and the like, and has certain application prospect.
Description
Technical Field
The invention belongs to the field of environment, and particularly relates to a method for preserving sulfate conjugates (sulfate conjugates) and glucuronic acid conjugates (glucuronides conjugates) in an urban sewage sample.
Background
Natural estrogen is a generic term for a class of sterols. There are up to 17 natural estrogens known at present, mainly comprising estrone (E1), estradiol (17 β -estradiol, E2) and estriol (E3), the basic role of which is to maintain the normal functioning of endocrine functions in humans and animals. In the last two decades, natural estrogens have gained widespread attention globally as a class of environmentally interfering chemicals. The natural estrogen in the environment is mainly excreted from human and animal bodies and is mainly excreted with urine. In order to effectively protect the water environment and improve the removal efficiency of the urban sewage treatment process on the natural estrogen, the method has no limit. The raw water of the sewage contains natural estrogen and natural estrogen combination, especially sulfate combination. In order to accurately evaluate the removal performance of a sewage treatment plant, the concentration of natural estrogen in sewage needs to be accurately measured. Under the action of aryl sulfatase (arylsulfatase) or glucuronidase (beta-glucuronidase), the natural estrogen sulfate conjugate and the glucuronic acid conjugate can be converted into corresponding natural estrogen. Therefore, in order to effectively maintain the integrity of the wastewater sample, it is necessary to effectively inhibit arylsulfatase and glucuronidase in the wastewater sample, i.e., to effectively preserve sulfate conjugates and glucuronide conjugates in the wastewater sample.
Generally, sewage samples are stored at a low temperature of 4 ℃ in most cases, but arylsulfatase and glucuronidase still exhibit high enzyme activities even at a low temperature of 4 ℃. There are also cases where mercury chloride, an inhibitor such as sodium azide or formaldehyde, or a low pH (<3) is added, but the effect is not preferable.
Disclosure of Invention
In view of the above problems, an object of the present invention is to provide a method for preserving sulfate ester bound bodies and glucuronic acid bound bodies in municipal sewage.
The purpose of the invention is realized by the following technical scheme:
a method for preserving sulfate conjugates and glucuronide conjugates in municipal sewage comprises the following steps:
and (3) taking a municipal sewage sample, and adjusting the pH value to 11-14.
Preferably, the pH is adjusted to 11.
Preferably, the pH is adjusted by adding an alkaline substance or a substance whose aqueous solution is alkaline.
Preferably, the alkaline substance is one or two of strong alkali and weak alkali.
Preferably, the strong base is NaOH, LiOH, KOH, Ca (OH)2And Ba (OH)2One kind of (1).
Preferably, the alkaline substance in the aqueous solution is Na2CO3、Na2S、NaHCO3、NaHS、K2CO3、KHCO3、K2S、CaHCO3And CH3COONa.
Compared with the prior art, the invention has the following advantages and beneficial effects:
the method has the advantages of simple operation, good effect, low price and the like, has better inhibiting effect on arylsulfatase and glucuronidase in the sewage, and can realize effective preservation of the sulfuric acid combination and the glucuronic acid combination in the sewage sample.
Drawings
FIG. 1 is a graph showing the trend of p-nitrophenol sulfate conjugate in the wastewater sample of example 1 with respect to the preservation time, wherein the inset is the linear identification of different preservation conditions of the wastewater sample, wherein pNPS represents the p-nitrophenol sulfate conjugate.
FIG. 2 is a graph showing the trend of p-nitrophenol glucuronic acid conjugate in the sewage sample of example 2 with respect to the preservation time, wherein the insert graph is a linear mark of different preservation conditions of the sewage sample, and pNPS represents the p-nitrophenol glucuronic acid conjugate.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the embodiments of the present invention are not limited thereto.
Examples the p-nitrophenol sulfate conjugate (purity > 98%) was purchased from Sigma Aldrich; the p-nitrophenol glucuronic acid conjugate (purity > 98%) was purchased from Sigma Aldrich; the sewage is raw water taken from sewage of a certain city in Guangzhou city; the room temperature is 25 ℃, but the experimental effect is not influenced by the operation at the temperature of 13-28 ℃.
The sewage contains a small amount of arylsulfatase and glucuronidase, but in order to verify the preservation effect of the invention and save the experimental time, extra p-nitrophenol sulfate ester combination and p-nitrophenol glucuronic acid combination are artificially added.
Example 1
Taking 4 sewage samples (20mL), adding the p-nitrophenol sulfate combination into each sewage sample according to the standard of 50 mu mol/L, and respectively preserving under the following conditions:
1. the pH of the sewage is 11 and the sewage is stored at room temperature;
a NaOH solution having a concentration of 0.5mol/L was added to the sewage sample so that the pH of the sewage sample became 11.
2. The pH value of the sewage is 1 and the sewage is stored at room temperature;
hydrochloric acid solution with the concentration of 1mol/L is added into the sewage sample, so that the pH value of the sewage sample is 1.
3. The pH of the sewage is not adjusted and is stored at room temperature;
4. the pH of the wastewater was not adjusted and stored at 4 ℃.
And measuring the content of the p-nitrophenol sulfate conjugate under different storage conditions at regular intervals, namely at the time of storing for 1h, 2h, 4h, 6h, 12h, 24h, 36h and 48h respectively, wherein the content of the p-nitrophenol sulfate conjugate is basically unchanged if the sample storage condition is good, and the content of the p-nitrophenol sulfate conjugate is continuously reduced along with the increase of the storage time.
The trend of the p-nitrophenol sulfate conjugate in the wastewater sample of example 1 with the preservation time is shown in FIG. 1, and it can be derived from FIG. 1: under the above 4 different sample storage conditions, only the storage condition of pH 11 exhibited a better storage effect.
Example 2
Taking 4 sewage samples (20mL), adding p-nitrophenol glucuronic acid combination into each sewage sample according to the standard of 50 mu mol/L, and respectively preserving under the following conditions:
1. the pH of the sewage is 11 and the sewage is stored at room temperature;
a NaOH solution having a concentration of 0.5mol/L was added to the sewage sample so that the pH of the sewage sample became 11.
2. The pH value of the sewage is 1 and the sewage is stored at room temperature;
hydrochloric acid solution with the concentration of 1mol/L is added into the sewage sample, so that the pH value of the sewage sample is 1.
3. The pH of the sewage is not adjusted and is stored at room temperature;
4. the pH of the wastewater was not adjusted and stored at 4 ℃.
The content of the p-nitrophenol glucuronic acid conjugate under different storage conditions is measured at regular intervals, namely at the time of storing for 1h, 2h, 4h, 6h, 12h, 24h, 36h and 48h respectively, if the storage condition of the sample is good, the content of the sample is basically unchanged, and otherwise, the content of the p-nitrophenol glucuronic acid conjugate is continuously reduced along with the increase of the storage time.
The trend of the p-nitrophenol glucuronic acid conjugate in the wastewater sample of example 2 with the preservation time is shown in FIG. 1, and it can be derived from FIG. 1: under the above 4 different sample storage conditions, only the pH 11 and pH 1 storage conditions exhibited good storage effects, but the sulfuric acid conjugate was partially hydrolyzed due to the pH 1 storage condition. Therefore, in order to ensure that both the sulfate conjugate and the glucuronide conjugate in the wastewater remain intact, pH 11 is an optimum storage condition.
Without being limited to the above embodiments, other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the invention should be construed as equivalents thereof and are intended to be included in the scope of the invention.
Claims (6)
1. A method for preserving sulfate conjugates and glucuronide conjugates in municipal sewage is characterized by comprising the following steps: and (3) taking a municipal sewage sample, adjusting the pH value to 11-14, and storing at room temperature.
2. The method for preserving sulfate conjugates and glucuronic acid conjugates in municipal sewage according to claim 1, wherein the pH is 11.
3. The method for preserving sulfate complex and glucuronic acid complex in municipal sewage according to claim 1, wherein the pH is adjusted by adding an alkaline substance or an aqueous solution thereof to make the pH alkaline.
4. The method for preserving sulfate conjugate and glucuronide conjugate in municipal sewage according to claim 3, wherein the alkaline substance is one or both of strong alkali and weak alkali.
5. The method as claimed in claim 4, wherein the strong alkali is NaOH, LiOH, KOH, Ca (OH)2And Ba (OH)2One kind of (1).
6. The method for preserving sulfate complex and glucuronic acid complex in municipal sewage according to claim 3, wherein the alkaline substance in the aqueous solution is Na2CO3、Na2S、NaHCO3、NaHS、K2CO3、KHCO3、K2S、CaHCO3And CH3COONa.
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| CN103063791A (en) * | 2012-12-06 | 2013-04-24 | 国家烟草质量监督检验中心 | Method of simultaneously determining contents of 1-OHP ,3-OHB[a]P and 3-OHB[a]A in urine |
| CN104903442A (en) * | 2013-01-09 | 2015-09-09 | 夏尔人类遗传性治疗公司 | Methods for purification of arylsulfatase a |
| CN109781876A (en) * | 2019-01-11 | 2019-05-21 | 云南中烟工业有限责任公司 | A method of utilizing benzo [a] pyrene in the Soxhlet extraction device detection smoker urine with Solid Phase Extraction function |
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2019
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Patent Citations (4)
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| CN101625310A (en) * | 2008-07-09 | 2010-01-13 | 中国科学院沈阳应用生态研究所 | Analysis method for detecting arylsulfatase activity in soil |
| CN103063791A (en) * | 2012-12-06 | 2013-04-24 | 国家烟草质量监督检验中心 | Method of simultaneously determining contents of 1-OHP ,3-OHB[a]P and 3-OHB[a]A in urine |
| CN104903442A (en) * | 2013-01-09 | 2015-09-09 | 夏尔人类遗传性治疗公司 | Methods for purification of arylsulfatase a |
| CN109781876A (en) * | 2019-01-11 | 2019-05-21 | 云南中烟工业有限责任公司 | A method of utilizing benzo [a] pyrene in the Soxhlet extraction device detection smoker urine with Solid Phase Extraction function |
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| "太湖水稻土中的芳基硫酸酯酶活性;陆琴 等;《土壤学报》;20030531;第386-392页 * |
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