Search

In recent years, with the increasingly serious problem of environmental pollution, people′s awareness of environmental protection has gradually strengthened. In addition to the monitoring of conventional pollutants such as heavy metals and pesticides, the monitoring scope has been extended to emerging contaminants (ECs), which have the potential to cause known or suspected adverse for ecological or human health effects. Recently, a new group of compounds has been added to the anthropological-based pollutants, which are illicit drugs. The main source of these residues is from consumers. After ingestion of the illicit drug dose, active parent compounds and their metabolites are excreted through urine, entering urban wastewater and reaching wastewater treatment plants (WWTPs). These substances may have low removal efficiencies and persist in the treated wastewater. Though the concentrations of emerging contaminants in environment are low, the risks for human health and environment cannot be excluded. Considering the serious threat posed by these substances, our country has clearly put forward the work deployment of “paying attention to the treatment of new pollutants”. Current analytical methods developed for the determination of trace level of compound in wastewater samples usually include pre-concentration steps, the most common being those based on solid-phase extraction (SPE) and online-SPE. However, there are many disadvantages of SPE, such as laborious, time-consuming, cost-consuming and needing specialized instrumentation. Therefore, the convenient and fast methods need to be developed, which can meet the high-sensitivity analysis requirements of wastewater detection. Here, a method of micro-direct-injection ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed for the rapid screening of 50 emerging contaminants. The wastewater samples were centrifuged at 13 500 r/min for 3 min, the supernatants were filtered through PTFE filters before injection into the UPLC-MS/MS system. A Waters Acquity UPLC HSS T3 column (100 mm×2.1 mm×1.8 μm) was used, the mobile phases were 5 mmol/L ammonium acetate-0.01% formic acid (A) and acetonitrile (B). The result showed that the limits of detection (LODs) of 50 targets were 0.1-5 ng/L, the extraction recovery was 65.4%-113.9%, and the matrix effect was 64.8%-139.8%. The methamphetamine, codeine, morphine, ketamine, tramadol, O-demethyltramadol and 2-fluoro-deschloroketamine were detected in the real wastewater sample. This method can rapidly and simply screen the trace amounts of a variety of emerging contaminants in wastewater samples.

Assessing collective drug consumption based on the species and concentrations of illicit drugs and their metabolites in wastewater is an objective, real-time, accurate, convenient and effective monitoring technology. In order to establish a rapid screening and confirmation method for the abuse of opioids, amphetamines and benzodiazepines in wastewater, solid phase extraction was used to pretreat the wastewater sample, and ultra-high liquid chromatography tandem high resolution mass spectrometry was used to screen and confirm 36 kinds of analytes. Moreover, the method was applied to real wastewater samples collected from different wastewater treatment plants. Different HPLC columns and mobile phases were tested for optimization of the method. The peak shapes, retention time, separation and sensitivity of the chromatographic procedure were evaluated. Finally, an Accucore Hypersil Gold column (100 mm×2.1 mm×1.9 μm), and the mobile phases of ultrapure water with 2 mmol/L ammonium formate 0.1%-formic acid (A) and acetonitrile-methanol (1∶1, V/V) with 2 mmol/L ammonium formate and 0.1% formic acid were applied because of good peak shapes and separation. TraceFinder software was selected for rapid screening, and retention time, molecular mass, fragment ions and isotope distribution were collected as the screening basis. A substance could be judged as positive if it all met these 4 screening conditions. Therefore, the results obtained were more authentic and reliable. The LODs ranged from 5 to 20 ng/L. The extraction recoveries were higher than 70% for all compounds in wastewater, and the matrix effect ranged from -24.4% to 21.2%. In the real wastewater samples, 4 opioids of morphine, codeine, pethidine, tramadol, 1 amphetamine of methamphetamine and 4 benzodiazepines of diazepam, nordazepam, estazolam, alprazolam were detected, and the error of all compounds were less than 5×10-6. There are many kinds of abused substances in wastewater, and the regional prevalence is also different. The method established in this article can be used for rapid and accurate screening and confirmation abused substances in wastewater.

In recent years, as the third-generation of drugs, new psychoactive substances （NPS） have expanded rapidly and become a serious concern for China’s anti-drug prevention and control system. As a new drug monitoring technology in the current anti-drug field, wastewater analysis is an objective, real-time, accurate, convenient and effective drug monitoring method. In recent years, it has gradually been applied to the monitoring of NPS. This study summarizes wastewater sample collection, target stability research, wastewater sample pretreatment, wastewater sample analysis methods, target NPS consumption calculations and actual monitoring applications, with a view to the construction of a monitoring system for NPS in wastewater, real-time and accurate grasp of information on the use of NPS in cities, the reflection of the actual consumption of different types of NPS and consumption trends in a short period of time, and prediction of the development trend of abused use, which is of great significance for combating NPS crimes, serving and guaranteeing the personal safety of the people, and maintaining social stability.

Objective: To determine the normal reference values of 33 elements, Ag, Al, As, Au, B, Ba, Be, Ca, Cd, Co, Cr, Cs, Cu, Fe, Ga, Hg, Li, Mg, Mn, Mo, Ni, Pb, Rb, Sb, Se, Sr, Th, Ti, Tl, U, V, Zn and Zr, in the blood and urine samples from the general population in Sanmen County of Zhejiang province, a typical coastal area of eastern China., Methods: The 33 elements in 272 blood and 300 urine samples were determined by inductively coupled plasma-mass spectrometry (ICP-MS). The normality test of data was conducted using SPSS 17.0 Statistics. The data was compared with other reports., Results: The normal reference values of the 33 elements in the blood and urine samples from the general population in Sanmen County were obtained, which of some elements were found to be similar with other reports, such as Co, Cu, Mn and Sr, while As, Cd, Hg and Pb were generally found to be higher than those previously reported. There was a wide variation between the reports from different countries in blood Ba., Conclusion: The normal reference values of the 33 elements in the blood and urine samples from the general population in Sanmen County are established, and successfully applied to two poisoning cases.

Objective: To establish the electricity plate digestion and inductively coupled plasma-mass spectrometry (ICP-MS) method for determination of 33 inorganic elements in human hair., Methods: Lithium (6Li), Germanium (72Ge), Yttrium (89Y), Indium (115In), and Terbium (159Tb) were used as internal standards. The electric heating board digestion in a mixture of nitric acid and hydrogen peroxide was used as the pre-treatment of the hair. Thirty-three inorganic elements in human hair were analyzed by ICP-MS method., Results: The detection limit of ICP-MS was 0.0001 microg/g(Th)-10.9 microg/g (Ca) and the limit of quantitation was 0.0005 microg/g (Th)-25 microg/g (Ca). The recovery rate of this method was 86%-113%. The RSD for the intra-day and inter-day were less than 9.2%. The method was not statistically different from microwave digestion method., Conclusion: This method is highly efficient and accurate. It can be used for analysis of 33 inorganic elements in human hair.

Objective: To establish the method for measurement of acetonitrile in blood and urine by head-space gas chromatography., Methods: DB-ALC1 (30 m x 320 microm x 1.8 microm) and DB-ALC2 (30 m x 320 microm x 1.2 microm) capillary column were used to measure the acetonitrile in blood and urine with the isopropanol as internal standard reference., Results: The limits of detection of acetonitrile in both blood and urine were 0.5 microg/mL, with a linear range of 5-1000 microg/mL (r = 0.999).The accuracy of this method was 93.2%-98.0%. The RSD for the intra-day and inter-day were less than 3.7%., Conclusion: The method is capable for measurement analysis of acetonitrile in blood and urine.