CN114577925A - Method for rapidly detecting fecal sterol substances in water sample - Google Patents

Method for rapidly detecting fecal sterol substances in water sample Download PDF

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CN114577925A
CN114577925A CN202111639733.6A CN202111639733A CN114577925A CN 114577925 A CN114577925 A CN 114577925A CN 202111639733 A CN202111639733 A CN 202111639733A CN 114577925 A CN114577925 A CN 114577925A
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CN114577925B (en
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孙玉川
沈立成
王永啟
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Abstract

The invention discloses a method for rapidly detecting a fecal sterol substance in a water sample, which is characterized in that according to the principle of gel permeation chromatography, macromolecular substances flow out of a column at first, and then micromolecular substances flow out of the column, and by utilizing the principle, the collection time of the effluent can be set according to the molecular weight of a target substance, and substances in a specific molecular weight region are collected, so that the purpose of purifying the sample is achieved. The standard recovery rate and the detection limit of the method are superior to those of the existing methods, in addition, according to different contents of the phytosterol substances in the water sample, the method is suitable for the water sample with the volume of 50-4000 mL, and can meet the analysis of the trace phytosterol substances in the water sample.

Description

Method for rapidly detecting fecal sterol substances in water sample
Technical Field
The invention relates to the technical field of environmental protection treatment, in particular to a method for rapidly detecting a phytosterol substance in a water sample.
Background
The coprosterol substance belongs to a steroid biomarker series, namely 5 beta-stanol configuration, and is a series of steroids formed by hydrogenation reduction conversion of ingested cholesterol and homologs thereof through a delta 5 double bond under the catalytic action of escherichia coli in intestines of higher animals. Therefore, the fecal sterol substance can be used as an indicator of human and various animal excreta and used for researching the source of sewage in surface water and underground water. China is a large country in population and agriculture and animal husbandry, and pollution caused by excrement of human beings, animal husbandry and the like causes pollution to surface water and underground water bodies of a plurality of places. More and more research is focused on the environmental indication characteristics of fecal sterols and their mechanism of influence.
In the research of the analytical method of the coprosterol, the pretreatment technology of the environmental sample mostly adopts the steps of liquid-liquid extraction or DEAE-cellulose extraction, concentration and column chromatography classification elution, the instrument detection technology is mostly determined by a gas chromatography-hydrogen flame detector (GC-FID), and the gas chromatography-mass spectrometry is rarely used for determination. The existing methods have the problems of large solvent waste, complex operation, low sample recovery rate, high detection cost and the like. In addition, when a sample is purified and separated, alumina, an acidic silica gel column and the like are mostly used, but most of the methods absorb the sample to be detected to different degrees, so that the recovery rate of the sample is reduced.
Disclosure of Invention
The invention aims to solve the problems and provide a method for rapidly detecting the fecal sterol substances in the water sample.
The invention realizes the purpose through the following technical scheme:
the invention comprises the following steps:
s1: filtering the collected sample, adding a recovery rate indicator into the filtered water sample, extracting by a solid phase extraction system, and collecting an extracting solution for later use;
s2: evaporating and drying the extracting solution, adding an ethyl acetate-cyclohexane mixed solvent, and removing macromolecular interferents and micromolecular interferents in the sample by using a gel purification and online concentration system;
s3: adding a silanization reagent into the concentrated sample, sealing and filling nitrogen for protection, heating, placing and cooling, and then placing into a refrigerator for freezing and storing to be tested by an upper machine;
s4: detecting a sample by adopting a gas chromatography-mass spectrometry combined system, simultaneously acquiring full scan data and selective ion scan data, performing qualitative analysis on the full scan data, performing quantitative analysis on the selective ion scan data, performing quantitative analysis on the phytosterol substance by using an internal standard method, and determining the content of the phytosterol substance by comparing the areas of a target peak and an internal standard peak in a selective ion chromatogram.
Preferably, in step S1, the collected sample is filtered, specifically, filtered by using a glass fiber membrane with an effective pore size of 0.7 μm.
Preferably, in step S1, the extraction membrane used in the solid-phase extraction system is a glass fiber-graphene oxide-polydimethylsiloxane composite membrane.
Further, in the step S2, evaporating and drying by using a rotary evaporator, wherein the volume ratio of ethyl acetate-cyclohexane is 1: 1; the parameter conditions of the gel purification and on-line concentration system are as follows: taking a sample volume of 2mL and an ethyl acetate-cyclohexane mixed solvent as a mobile phase, collecting fractions with a retention time of 4.5-8.6 min at a flow rate of 4.7mL/min, wherein the molecular weight of the fractions in the time period is 350-450, and the fractions contain all the phytosterols; concentrating to 200 μ L on line; add 5 ug/ul internal standard deuterated cholesterol 2 ul.
Preferably, the silylation agent in the step S3 is N, O-bis (trimethylsilyl) trifluoroacetamide, the adding amount is 60 μ L, the heating condition is 70 ℃, and the heating time is 2 h.
Specifically, the detection conditions of the gas chromatography-mass spectrometry system in step S4 are as follows: the chromatographic column is an HP-5MS capillary column with the volume of 30.0m multiplied by 0.32mm multiplied by 0.25 mu m, the carrier gas is high-purity helium, the flow rate is 1mL/min, the injection port temperature is 280 ℃, the temperature rising procedure is 50 ℃ at the initial temperature, the temperature is raised to 200 ℃ at 20 ℃/min after being kept for 1min, then the temperature is raised to 290 ℃ at the speed of 10 ℃/min, the temperature is kept for 15min, and the sample feeding amount is 1 mu L; EI ionization source 70eV, ion source temperature 230 ℃.
The invention has the beneficial effects that:
the invention relates to a method for rapidly detecting a phytosterol substance in a water sample, which is superior to the prior methods in the aspects of standard recovery rate and detection limit, and is suitable for the water sample with the volume of 50-4000 mL according to different contents of the phytosterol substance in the water sample, and can meet the analysis of trace amounts of the phytosterol substance in the water sample.
Drawings
FIG. 1 is a total ion current chromatogram of a fecal sterol substance in an underground river outlet water sample of an old dragon cave in southern Chongqing according to an embodiment of the invention.
In the figure: 1. deuterated nonadecanol, 2, copriol, 3, epimeric copriol, 4, coprone, 5, deuterated cholesterol, 6, cholesterol, 7, dihydrocholesterol, 8, 24-ethyl-copriol, 9, 24-ethyl-cholesterol, 10, stigmasterol, 11, sitosterol.
Detailed Description
The invention will be further described with reference to the accompanying drawings in which:
the invention adopts a full-automatic solid phase extraction system to extract the fecterols in the water sample, thereby avoiding the defects of low liquid-liquid extraction efficiency, high cost and labor waste. Macromolecular substances such as pigments and proteins in the extracting solution can influence the vaporization of a target object, and organic sulfur of small molecules can cause the corrosion of an instrument and influence the precision and the sensitivity of the instrument. According to the principle of gel permeation chromatography, macromolecular substances flow out of the column at first, and then small molecular substances flow out of the column, and by utilizing the principle, the collection time of effluent can be set according to the molecular weight of a target object, and substances in a specific molecular weight region can be collected, so that the purpose of purifying a sample is achieved. In addition, the coprosterol substance has various isomers, and the substances have higher boiling point, melting point and solubility, are difficult to separate and have more interference. But the molecular weights of the substances are similar, so that the gel purification system can collect fractions in a narrower time period, and the interference of other substances can be better eliminated.
The reagent materials, instruments and equipment used in the invention and the method have the following specific processes:
reagents and materials
The normal hexane, dichloromethane, methanol, ethyl acetate and cyclohexane used for sample analysis are purchased from Fisher company of America and are all high performance liquid chromatography pure. Glass fiber membranes (Whatman GF/F, effective pore size 0.7 μm) were fired in a muffle furnace at 450 ℃ for 6 h.
Second, sample extraction and purification
Sample extraction:
the collected sample is firstly filtered by a glass fiber membrane with the effective aperture of 0.7 mu m, 1L of the filtered water sample is filled into a brown bottle, and a recovery rate indicator is added. The extraction was performed using a fully automated solid phase extraction system (SPE-DEX 4790, horizons, USA) using a glass fiber-graphene oxide-polydimethylsiloxane composite membrane, and the extract was collected in a 60mL heart-shaped flask. The solid phase extraction scheme is shown in Table 1.
TABLE 1 full-automatic solid phase extraction procedure
Solvent(s) soak time dry time
Prewet1 N-hexane 1:30 1:30
prewet2 Methanol 1:30
prewet3 Ultrapure water 1:30
Airdry 5:00
Rinse1 Methanol water ═ 9:1(v/v) 1:30 1:00
Rinse2 Methylene dichloride 1:30 1:00
Rinse3 Methylene dichloride 0:45 2:00
Rinse4 Methylene dichloride 0:45 1:00
Rinse5 Methylene dichloride 1:30 2:00
Purifying an extracting solution:
the extraction solution was evaporated to dryness by rotary evaporation, 2mL of a mixed solvent of ethyl acetate-cyclohexane (1:1, V/V) was added, and the mixture was transferred to a 5mL sample bottle. And removing macromolecular interferents such as pigment and protein and some micromolecular interferents in the sample by using a gel purification and online concentration system (J2 AccuPrep MPS + AccuVap GPC).
The gel purification conditions were: adopting a Bio-Beads SX3 rapid column for purification, wherein the sample volume is 2mL, an ethyl acetate-cyclohexane (1:1, V/V) mixed solvent is used as a mobile phase, the flow rate is 4.7mL/min, collecting fractions with the retention time of 4.5-8.6 min, and the molecular weight of the fractions in the time period is about 350-450, and the fractions contain all the phytosterol substances. Concentrate to 200. mu.L in-line. Add 2 μ L of deuterated cholesterol (5 μ g/μ L) as internal standard.
The concentrated sample is added with 60 μ L of silylation reagent N, O-bis (trimethylsilyl) trifluoroacetamide (BSTFA), sealed and protected by nitrogen, heated for 2h at 70 ℃ and left overnight. After the sample is cooled, the sample is put into a refrigerator for freezing and storing until the sample is tested by the upper machine.
Thirdly, detecting the fecal sterol substance
The detection of the coprosterol substance adopts a gas chromatography-mass spectrometry combined system (GC-MS) for analysis (Agilent, 7890A/5975C), and a chromatographic column is an HP-5MS capillary column (30.0m multiplied by 0.32mm multiplied by 0.25 mu m). The carrier gas is high-purity helium, the flow rate is 1mL/min, the injection port temperature is 280 ℃, the temperature rising procedure is that the initial temperature is 50 ℃, the temperature is raised to 200 ℃ at 20 ℃/min after the temperature is maintained for 1min, then the temperature is raised to 290 ℃ at the speed of 10 ℃/min, and the temperature is maintained for 15 min. No split flow is used for sample injection, and the sample injection amount is 1 mu L. EI ionization source 70eV, ion source temperature 230 ℃. Full scan data and select ion scan data were collected simultaneously, qualitative (in contrast to the substance in the NIST11 mass library) with full scan data, and quantitative with select ion scan data. And (3) quantifying the phytosterol substance by using an internal standard method, and comparing the areas of a target peak and an internal standard peak in the selected ion chromatogram to determine the content of the phytosterol substance.
Fourth, the detection result
Since the coprosterol substance has no pure standard substance and the recovery rate and the detection limit of the method cannot be inspected by each target object, the method adopts the deuterated nonadecanol and the deuterated cholesterol to inspect the recovery rate and the detection limit of the sample. Preparing 1L of mixed solution of deuterated nonadecanol and deuterated cholesterol with the concentration of 1000ng/L, extracting, purifying, concentrating, silanizing, and detecting by an instrument, and then calculating the recovery rate of the deuterated nonadecanol and the deuterated cholesterol. After 10 repeated experiments, the recovery rates of the deuterated nonadecanol and the deuterated cholesterol are 95.7 +/-5.3 percent and 93.2 +/-6.8 percent, which are far superior to the recovery rate of liquid-liquid extraction, and the detection limits of the deuterated nonadecanol and the deuterated cholesterol are 0.5ng/L and 1.2ng/L respectively. The method is proved to have good repeatability, accuracy and reliability.
By using the method, water samples such as an underground river of an old dragon cave in Chongshan mountain, an underground river of a Qingmu guan and a Tansha Tan river in Jinfo mountain are detected, and the detected fecal sterol substances mainly comprise: coproanol, differentially purchased coproanol, 24-ethyl-differentially purchased coproanol, cholesterol, dihydrocholesterol, coprostanone, dihydrocholesterol, 24-ethyl-coproanol, 24-ethyl-dihydrocholesterol, sitosterol, stigmasterol. The names and characteristic ions of the detected coprosterols are shown in the table 2.
FIG. 1 is a total ion current chromatogram of a fecal sterol substance in an underground river outlet water sample of an old dragon cave in southern Chongqing. As can be seen from figure 1, the fecal sterol substances detected in the water sample of the underground river outlet of the old dragon cave in the south Chongqing mountain are mainly as follows: 9 kinds of coprosterol substances such as coprosterol, epimeric coprostanol, fecal ketone, cholesterol, dihydrocholesterol, 24-ethyl-coprostanol, 24-ethyl-cholesterol, stigmasterol, sitosterol and the like.
Table 2 names and characteristic ions of the fecal sterols
Figure BDA0003443108220000061
Figure BDA0003443108220000071
The foregoing shows and describes the general principles and features of the present invention, together with the advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (6)

1. A method for rapidly detecting a phytosterol substance in a water sample is characterized by comprising the following steps:
s1: filtering the collected sample, adding a recovery rate indicator into the filtered water sample, extracting by a solid phase extraction system, and collecting an extracting solution for later use;
s2: evaporating and drying the extracting solution, adding an ethyl acetate-cyclohexane mixed solvent, and removing macromolecular interferents and micromolecular interferents in the sample by using a gel purification and online concentration system;
s3: adding a silanization reagent into the concentrated sample, sealing and filling nitrogen for protection, heating, placing and cooling, and then placing into a refrigerator for freezing and storing to be tested by an upper machine;
s4: detecting a sample by adopting a gas chromatography-mass spectrometry combined system, simultaneously acquiring full scan data and selective ion scan data, performing qualitative analysis on the full scan data, performing quantitative analysis on the selective ion scan data, performing quantitative analysis on the phytosterol substance by using an internal standard method, and determining the content of the phytosterol substance by comparing the areas of a target peak and an internal standard peak in a selective ion chromatogram.
2. The method for rapidly detecting the fecal sterol substance in the water sample according to claim 1, wherein the method comprises the following steps: in step S1, the collected sample is filtered, specifically, a glass fiber membrane with an effective pore size of 0.7 μm is used for filtering.
3. The method for rapidly detecting the fecasterol substances in the water sample according to claim 1, which is characterized in that: in the step S1, the extraction membrane used by the solid-phase extraction system is a glass fiber-graphene oxide-polydimethylsiloxane composite membrane.
4. The method for rapidly detecting the fecal sterol substance in the water sample according to claim 1, wherein the method comprises the following steps: in the step S2, evaporating and drying by using a rotary evaporator, wherein the volume ratio of ethyl acetate to cyclohexane is 1: 1; the parameter conditions of the gel purification and on-line concentration system are as follows: taking a sample volume of 2mL and an ethyl acetate-cyclohexane mixed solvent as a mobile phase, collecting fractions with a retention time of 4.5-8.6 min at a flow rate of 4.7mL/min, wherein the molecular weight of the fractions in the time period is 350-450, and the fractions contain all the phytosterols; concentrating to 200 μ L on line; add 5 ug/ul of internal standard deuterated cholesterol 2 ul.
5. The method for rapidly detecting the fecasterol substances in the water sample according to claim 1, which is characterized in that: in the step S3, the silylation agent is N, O-bis (trimethylsilyl) trifluoroacetamide, the adding amount is 60 mu L, the heating condition is 70 ℃, and the heating time is 2 h.
6. The method for rapidly detecting the fecal sterol substance in the water sample according to claim 1, wherein the method comprises the following steps: the detection conditions of the gas chromatography-mass spectrometry system in the step S4 are as follows: the chromatographic column is an HP-5MS capillary column with the thickness of 30.0m multiplied by 0.32mm multiplied by 0.25 mu m, the carrier gas is high-purity helium, the flow rate is 1mL/min, the injection port temperature is 280 ℃, the temperature rise program is 50 ℃ of the initial temperature, the temperature is raised to 200 ℃ at 20 ℃/min after being maintained for 1min, then the temperature is raised to 290 ℃ at the speed of 10 ℃/min, the temperature is maintained for 15min, and the sample injection amount is 1 mu L; EI ionization source 70eV, ion source temperature 230 ℃.
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