Citation: HUANG Qing, HU Sheng-Hua, YANG Dao-Bing, WANG Xiao-Ru, XING Jun. Determination of Four Kinds of Illicit Drugs in Wastewater by Micro-extraction Tube Injection Coupled with Gas Chromatography-Tandem Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, ;2022, 50(1): 153-161. doi: 10.19756/j.issn.0253-3820.210687 shu

Determination of Four Kinds of Illicit Drugs in Wastewater by Micro-extraction Tube Injection Coupled with Gas Chromatography-Tandem Mass Spectrometry

1.
College of Chemistry and Molecular Sciences, Wuhan University, Wuhan 430072, China;
2.
Judicial Drug Identification Center, Wuhan City Public Security, Wuhan 430010, China

Corresponding author: XING Jun, gc-ms@263.net
Received Date: 18 August 2021
Revised Date: 22 November 2021

Micro-extraction tube injection (METI), a needle-typed micro-extraction technology, has been proposed for gas chromatography (GC). In METI, a section of monolithic capillary tube (5 cm in length) works as an extraction tube and also as an injection needle. Based on the strategy of static desorption in tube and direct injection with tube, METI is able to enrich analytes at ng/L level in water for GC analysis when 1 mL of sample is consumed. In this work, the monolithic capillary tube was prepared with N-vinylpyrrolidone (NVP) and divinylbenzene (DVB), and four kinds of illicit drugs including methamphetamine, ketamine, norketamine and cocaine were tested. After the conditions of METI were optimized, a method of METI coupled with gas chromatography-tandem mass spectrometry (GC-MS/MS) was established for determination of illicit drugs in wastewater. The linear ranges were 0.05-50 μg/L for methamphetamine, ketamine and norketamine, and 0.10-50 μg/L for cocaine with the correlation coefficients (R²) greater than 0.9985. The limits of detection (S/N=3) of the analytes varied from 0.32 to 10.00 ng/L, and the limits of quantification (S/N=10) were in the range of 1.07-33.00 ng/L. The spiking recoveries ranged from 74.65% to 114.36% at spiking levels of 0.3, 3.0 and 30.0 μg/L in water samples from East Lake and intake of wastewater treatment plant, and relative standard deviations (RSDs) were less than 10.6%, except for cocaine which was 15.0% at low concentration in East Lake water. METI integrated separation, enrichment and injection, with the advantages including simple operation and high enrichment efficiency, and could be used for rapid pretreatment of trace components in small amounts of samples.
- Sample pretreatment,
- Micro-extraction tube injection,
- Illicit drugs,
- Wastewater,
- Gas chromatography-tandem mass spectrometry
1. [1]
  LAI F Y, BRUNO R, LEUNG H W, THAI P K, ORT C, CARTER S,THOMPSON K, LAM P K S, MUELLER J F. Forensic Sci. Int., 2013, 233(1):126-132.
2. [2]
  KHAN U, VAN NUIJS A L N, LI J, MAHO W, DU P, LI K Y, HOU L L, ZHANG J Y, MENG X Z, LI X Q, COVACI A. Sci. Total Environ., 2014, 487:710-721.
3. [3]
  DU P, LI K Y, LI J, XU Z Q, FU X F, YANG J, ZHANG H F, LI X Q. Water Res., 2015, 84:76-84.
4. [4]
  LI K Y, DU P, XU Z Q, GAO T T, LI X Q. Environ. Pollut., 2016, 213:395-402.
5. [5]
  LIU S Y, YU W J, WANG Y R, SHAO X T, WANG D G. Environ. Sci. Pollut. Res., 2021, 28(13):16754-16766.
6. [6]
  DAUGHTON C G. ACS Symp. Ser., 2001, 791:348-363.
7. [7]
  MASTROIANNI N, BLEDA M J, DE ALDA M L, BARCELÓ D. J. Hazard. Mater., 2016, 316:134-142.
8. [8]
9. [9]
  RACAMONDE I, RODIL R, BENITO QUINTANA J, CELA R. Anal. Chim. Acta, 2013, 770:75-84.
10. [10]
  MORENO I, BARROSO M, MARTINHO A, CRUZ A, GALLARDO E. J. Chromatogr. B:Anal. Technol. Biomed. Life Sci., 2015, 1004:67-78.
11. [11]
  RACAMONDE I, VILLAVERDE-DE-SÁA E, RODIL R, BENITO QUINTANA J, CELA R. J. Chromatogr. A, 2012, 1245:167-174.
12. [12]
  MWENESONGOLE E M, GAUTAM L, HALL S W, WATERHOUSE J W, COLE M D. Anal. Methods, 2013,5(13):3248-3254.
13. [13]
  GONZÁLEZ-MARIÑO I, QUINTANA J B, RODRÍGUEZ I, CELA R. J. Chromatogr. A, 2010, 1217(11):1748-1760.
14. [14]
  ZHANG X H, HUANG R H, LI P, REN Y, GAO J F, MUELLER J F, THAI P K. Environ. Sci. Pollut. Res., 2019, 26(23):23593-23602.
15. [15]
16. [16]
  HU P, GUO C S, ZHANG Y, LV J P, ZHANG Y, XU J. Front. Environ. Sci. Eng., 2019, 13(4):56.
17. [17]
  SENTA I, KRIZMAN I, AHEL M, TERZIC S. Anal. Bioanal. Chem., 2013, 405(10):3255-3268.
18. [18]
  GONZALEZ-MARINO I, ESTEVEZ-DANTA A, RODIL R, MANUELA DA SILVA K, FABRIZ SODRE F, CELA R, BENITO QUINTANA J. Drug Test. Anal., 2019, 11(7):1018-1027.
19. [19]
  SENTA I, KRIZMAN I, AHEL M, TERZIC S. J. Chromatogr. A, 2015, 1425:204-212.
20. [20]
  LIN A Y C, LEE W N, WANG X H. Water Res., 2014, 53:351-360.
21. [21]
  MUSSHOFF F, LACHENMEIER D W, KROENER L, MADEA B. J. Chromatogr. A, 2002, 958(1):231-238.
22. [22]
23. [23]
  XING J, YE X Y, HUANG W Y. European Patent, 18788140.4, 2021.
24. [24]
25. [25]
26. [26]
  YAO W X, FAN Z F, ZHANG S L. J. Chromatogr. A, 2016, 1465:55-62.
27. [27]
  XIONG J, CHEN J, HE M, HU B. Talanta, 2010, 82(3):969-975.
28. [28]
  ISENSCHMID D S, LEVINE B S, CAPLAN Y H. J. Anal. Toxicol., 1989, 13(5):250-256.
29. [29]
  WANG H Q, ZHANG H H, WEI S G, JIA Q. J. Chromatogr. A, 2018, 1566:23-31.
30. [30]
  PANG J L, LIAO Y M, HUANG X J, YE Z W, YUAN D X. Talanta, 2019, 199:499-506.
31. [31]
  WONGNIRAMAIKUL W, CHOODUM A, DENNANY L, DAEID N N. J. Sep. Sci., 2012, 35(23):3332-3339.
32. [32]
  DJOZAN D J, BAHERI T, POURNAGHI-AZAR M H. Chromarographia, 2007, 65:45-50.
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