CN-122017077-A - Method for determining xanthate compound in soil

CN122017077ACN 122017077 ACN122017077 ACN 122017077ACN-122017077-A

Abstract

The invention belongs to the technical field of pollutant determination, and relates to a method for determining xanthate compounds in soil, which comprises the following steps of S1, freeze-drying soil to be tested, grinding and sieving, adding an extractant, oscillating and centrifuging, and taking supernatant; adding a purifying agent into the supernatant to perform dispersion solid phase extraction, filtering the supernatant after centrifugation, taking filtrate, adjusting pH for standby measurement, and S2, measuring the content of xanthate compounds in the filtrate by adopting a high performance liquid chromatography-tandem mass spectrometry method. The method has high recovery rate, good precision, high sensitivity and complex matrix interference resistance, is suitable for simultaneous determination of different xanthate compounds (ethyl xanthate EtX), (isopropyl xanthate IpX) and (butyl xanthate, buX) in soil with different physicochemical properties, and provides an efficient solution for developing research on pollution characteristics and risk levels of the xanthate compounds in complex soil.

Inventors

XIANG LEI
MO CEHUI
LI YANWEN
ZHAO HAIMING
WANG YIBO
ZHANG YU
CAI QUANYING
FENG NAIXIAN
LIU BAILIN

Assignees

暨南大学

Dates

Publication Date: 20260512
Application Date: 20260313

Claims (10)

1. A method for determining xanthate compounds in soil comprising the steps of: S1, freeze-drying soil to be tested, grinding, sieving, adding an extractant, vibrating and centrifuging to obtain a supernatant, adding a purifying agent into the supernatant for dispersion and solid phase extraction, centrifuging, filtering the supernatant, and regulating the pH value of the filtrate for standby measurement; s2, measuring the content of xanthate compounds in the filtrate by adopting a high performance liquid chromatography-tandem mass spectrometry method.
2. The method for determining xanthate compounds in soil according to claim 1, wherein the extractant is at least one of methanol, acetonitrile, water, and ammonia water, and the scavenger is at least one of C 18 , graphite carbon black, and N-propylethylenediamine.
3. The method for determining xanthate compounds in soil according to claim 1, wherein the extractant is a mixed solution of ammonia water and methanol, the addition amount of the extractant is 30% -50%, the extractant is a mixture of methanol and ammonia water, the volume ratio of the ammonia water to the methanol is 30-40:70-100, and the extractant is subjected to ultrasonic extraction for 2-4 times.
4. The method for determining xanthate compounds in soil according to claim 1, wherein the amount of the scavenger added is 5-10 mg/mL.
5. The method for determining xanthate compounds in soil according to claim 1, wherein the shaking condition is that the rotating speed is 2500-3500 rpm, the shaking time is 8-15min, and the centrifuging condition is that the rotating speed is 6000-8000 rpm, and the centrifuging time is 10-20 min.
6. The method for determining xanthate compounds in soil according to claim 1, wherein the filter membrane material during the filtration process is selected from at least one of PTFE, PES, PA and GHP, and the filter membrane has a pore size of 0.22 μm.
7. The method for determining xanthate compounds in soil according to claim 1, wherein the pH is 6.5-11, and formic acid is added for adjustment during the adjustment of the pH.
8. The method for determining xanthate compounds in soil according to claim 1, wherein the high performance liquid chromatography tandem mass spectrometry is adopted, wherein the chromatography conditions are that an HPH-C18 column is adopted as a chromatographic column, a mobile phase A is methanol solution, a mobile phase B is ammonia water solution, the sample injection amount is 5-8 mu L, the column flow rate is 300-400 mu L/min, the gradient elution procedure is that 100% mobile phase B is initially used, the mobile phase B is kept 1~1.5 min,1.1~1.5 min to be reduced to 0% mobile phase B, the mobile phase B is kept for 2.9-3 min, 4.1-4.5 min is recovered to 100% mobile phase B, target pollutants are eluted within 5-min, and the total running time is 10-12 min; The mass spectrum condition is that a negative ESI source is used as an ionization source, the ESI has the working condition and parameters that the spraying voltage is-4500V, the air curtain air pressure is 30 psi, the atomization air pressure is 60 psi, the drying air temperature is 500 ℃, and the monitoring mode is multiple reaction monitoring.
9. The method of determining xanthate compounds in soil of claim 1, wherein the xanthate compounds are at least one of ethyl xanthate, isopropyl xanthate, and butyl xanthate.
10. The method for determining xanthate compounds in soil according to claim 1, wherein the detection limit of the xanthate compounds is 0.05-0.72 μg/kg and the standard recovery rate is 73.2% -104.9%.

Description

Method for determining xanthate compound in soil Technical Field The invention relates to the technical field of soil pollutant detection, in particular to a method for determining xanthate compounds in soil. Background Xanthates (Xanthates) are a class of sulfur-containing organic compounds widely used as flotation collectors in mine flotation processes to effect separation of target minerals by adsorption onto the mineral surfaces. However, its use in large quantities results in residual xanthates entering the surrounding soil environment through waste water discharge, tailings stacking and the like. Research shows that xanthate is easy to decompose into toxic byproducts such as carbon disulfide, alcohols and the like in soil, has remarkable inhibition effect on soil microbial activity, nitrogen circulation and crop growth, and threatens human health even through a food chain. For example, ethyl xanthate (EtX) and isopropyl xanthate (IpX) have been shown to inhibit the growth and activity of thiobacillus ferrooxidans, with increasing amounts of which the inhibition of the strain is also progressively enhanced. The research shows that the xanthate compound has obvious interference effect on salmonidae fish embryo development and teratogenic effect on grass carp embryo and ovum at the concentration of 30 mug/L. It follows that the xanthate compound is a bioteratogen. Butyl xanthate (BuX) is more hydrophobic and is more likely to remain permanently in the soil and migrate to the groundwater system. Xanthate compounds may accumulate in soil or aquatic organisms and be transported and amplified by the food chain, creating a potential hazard to humans. Long-term exposure can lead to the accumulation of toxins in organisms, affecting the growth, proliferation and survival of the organisms. Xanthate compounds are also potent inhibitors of some mammalian cytochrome CYP isoforms (i.e., rat CYP2B1 and human CYP2B 6) and selective mechanism inactivating agents. Xanthate compounds, when bound to enzymes (inhibit enzymes), catalyze the conversion to active intermediates that are inactive by covalent post-binding to enzyme molecules. When the concentration of the drug injected into the body of the rat is 1 mg/kg, the thrombin content in the body is reduced, and the reflex activity is blocked when the concentration is 10 mg/kg. Quantitative structure-activity relationship analysis results show that the inactivation efficiency of the xanthate compound is related to the chemical structure of the xanthate compound, and the inactivation efficiency of the xanthate compound with longer alkyl chains or more branched chains is higher. Second, carbon disulphide with neurotoxicity can be decomposed under the condition of weak acid. Carbon disulphide can enter the brain through the blood, causing a disorder in the nervous system. More importantly, the existing mine soil pollution site exceeding rate is 33.4%, the dosage of the flotation agent is continuously increased, and residues of the flotation agent can damage the soil structure, inhibit microbial activity (such as nitrifying bacteria) and possibly threaten human health through crop accumulation. However, xanthate is easy to combine with organic matters and metal ions in soil, the existing analysis method is severely interfered by sulfur-containing compounds, trace accurate measurement is difficult to realize, and related environmental behaviors and ecological risk research are seriously lagged. Therefore, a reliable and efficient analysis method needs to be established to accurately evaluate the pollution condition, reveal the environmental trend of the flotation organic medicament, effectively control the risk of the flotation organic medicament in the soil ecosystem and ensure the ecological environment safety and the human health. Disclosure of Invention The invention provides a method for determining xanthate compounds in soil, which is based on DSPE-HPLC/MS-MS, omits complicated SPE procedures to simplify sample preparation, and realizes simultaneous extraction and determination of three xanthates in soil. In a first aspect, the present invention provides a method for determining xanthate compounds in soil comprising the steps of: S1, freeze-drying soil to be tested, grinding, sieving, adding an extractant, vibrating and centrifuging to obtain a supernatant, adding a purifying agent into the supernatant for dispersion and solid phase extraction, centrifuging, filtering the supernatant, and regulating the pH value of the filtrate for standby measurement; s2, measuring the content of xanthate compounds in the filtrate by adopting a high performance liquid chromatography-tandem mass spectrometry method. Preferably, the extractant is at least one of methanol, acetonitrile, water and ammonia water, and the purifying agent is at least one of C 18, graphite carbon black and N-propyl ethylenediamine. Preferably, the extractant is a mixed solution of ammonia water and methanol, t