PMID- 34213261
OWN - NLM
STAT- MEDLINE
DCOM- 20210727
LR  - 20210727
IS  - 1872-2059 (Electronic)
IS  - 1000-8713 (Linking)
VI  - 38
IP  - 12
DP  - 2020 Dec 8
TI  - [Determination of eight environmental phenols in human urine samples by 
      high-throughput solid-phase extraction-ultra-performance liquid 
      chromatography-tandem mass spectrometry].
PG  - 1456-1464
LID - 10.3724/SP.J.1123.2020.07021 [doi]
AB  - A method combining 96-well plate solid-phase extraction with ultra-performance 
      liquid chromatography-tandem mass spectrometry (96-well SPE LC-MS/MS) was 
      developed for the simultaneous determination of eight environmental phenols in 
      urine samples. The samples included seven bisphenol compounds and triclosan. The 
      urine samples were thawed to room temperature, and the target analytes were 
      deconjugated by beta -glucuronidase/aryl-sulfatase in ammonium acetate buffer 
      solution at 37℃ overnight. Then, the effects of three kinds of 96-well 
      solid-phase extraction plates and different elution conditions on the 
      purification of the urine samples and the environmental phenol recoveries were 
      compared. The best purification effect was achieved on Oasis HLB 96-well plate 
      (60 mg) solid phase extraction, using 30% (v/v) acetonitrile aqueous solution as 
      the rinse solution. The target analytes were then eluted by methanol solution and 
      evaporated to dryness using a nitrogen blower. After reconstruction with 0.5 mL 
      methanol/water (1:1, v/v) solution, the target compounds were detected by 
      UPLC-MS/MS. To achieve better chromatographic separation, two kinds of analytical 
      columns (C(18) and T3) and different types of mobile phases (methanol and 
      acetonitrile as the organic phase) were also compared. The best chromatographic 
      effect was achieved when the treated samples were separated on a C(18) column 
      (100 mmx2.1 mm, 1.7 mum) using acetonitrile/water as the mobile phase at a flow 
      rate of 0.3 mL/min. Mass spectra were recorded by negative electrospray 
      ionization under the multiple reaction monitoring (MRM) mode. The sample matrix 
      effect was also evaluated. The absolute matrix effects of bisphenol A, bisphenol 
      F, bisphenol S, bisphenol B, and bisphenol AF were in the range of 3.47% to 
      15.32%. Since the above mentioned matrix effect was weak, there was no need for 
      compensation measures. On the contrary, tetrachlorobisphenol A, 
      tetrabromobisphenol A, and triclosan showed an absolute matrix effect of 49.58% 
      (moderate), 71.99% (strong), and 86.93% (strong), thus necessitating compensation 
      measures. Therefore, this strategy uses a one-to-one corresponding isotope 
      internal standard method to offset the matrix effect. Six different urine samples 
      were used to evaluate the relative matrix effect. The relative standard 
      deviations (RSDs) of the eight corresponding internal standard peak areas were 
      3.63%-9.06%, indicating that the relative matrix effect was stable. Under the 
      optimized conditions, linearity ranges were 0.50-50 mug/L for bisphenol A and 
      bisphenol AF; 0.05-50 mug/L for tetrachlorobisphenol A and bisphenol S; 0.01-50 
      mug/L for bisphenol F and tetrabromobisphenol A; 1.00-50 mug/L for bisphenol B; and 
      5.00-200 mug/L for triclosan. The correlation coefficients were all greater than 
      0.9995. At spiked levels of 2.5, 5, and 25 mug/L, the average recovery ratios of 
      the eight target analytes were 81.01%-118.84%, while the intra-day and inter-day 
      precisions were 0.38%-19.41% and 2.54%-17.83%, respectively. The limits of 
      detection (LOD) were 0.002-1.09 mug/L, and the limits of quantitation (LOQ) were 
      0.007-3.63 mug/L. This method was successfully applied to the determination of the 
      eight environmental phenols in 64 urine samples collected from Beijing area 
      between 2019 and 2020. All the target environmental phenols were detected, except 
      for bisphenol B and bisphenol AF. Bisphenol A and bisphenol S showed the highest 
      detection rates of 100% and 96.9%, respectively. The detection rates of 
      triclosan, tetrabromobisphenol A, tetrachlorobisphenol A, and bisphenol F were 
      57.8%, 46.9%, 23.4%, and 21.9%, respectively. The medium values of urinary 
      concentration followed the order 1.44 mug/L(triclosan), 0.69 mug/L(bisphenol A), 
      0.086 mug/L (bisphenol S), 0.0032 mug/L (tetrabromobisphenol A), 0.00050 mug/L 
      (tetrachlorobisphenol A), 0.00 mug/L (bisphenol F, bisphenol B, and bisphenol AF). 
      The aforementioned results imply that the widespread environmental phenolic 
      exposure of Beijing residents is worthy of attention. Compared with traditional 
      solid-phase extraction methods, the method reported in this paper is time-saving, 
      effective, and suitable for the simultaneous analysis of large quantities of 
      samples; moreover, the small sample and organic solvent consumption make this 
      method more environment- and operator-friendly.
FAU - Lin, Xiao
AU  - Lin X
AD  - China CDC Key Laboratory of Environment and Population Health, National Institute 
      of Environmental Health, Chinese Center for Disease Control and Prevention, 
      Beijing 100021, China.
FAU - Qiu, Tian
AU  - Qiu T
AD  - China CDC Key Laboratory of Environment and Population Health, National Institute 
      of Environmental Health, Chinese Center for Disease Control and Prevention, 
      Beijing 100021, China.
FAU - Zhang, Xu
AU  - Zhang X
AD  - China CDC Key Laboratory of Environment and Population Health, National Institute 
      of Environmental Health, Chinese Center for Disease Control and Prevention, 
      Beijing 100021, China.
FAU - Hu, Xiaojian
AU  - Hu X
AD  - China CDC Key Laboratory of Environment and Population Health, National Institute 
      of Environmental Health, Chinese Center for Disease Control and Prevention, 
      Beijing 100021, China.
FAU - Yang, Yanwei
AU  - Yang Y
AD  - China CDC Key Laboratory of Environment and Population Health, National Institute 
      of Environmental Health, Chinese Center for Disease Control and Prevention, 
      Beijing 100021, China.
FAU - Zhu, Ying
AU  - Zhu Y
AD  - China CDC Key Laboratory of Environment and Population Health, National Institute 
      of Environmental Health, Chinese Center for Disease Control and Prevention, 
      Beijing 100021, China.
LA  - chi
PT  - Journal Article
PL  - China
TA  - Se Pu
JT  - Se pu = Chinese journal of chromatography
JID - 9424804
RN  - 0 (Phenols)
SB  - IM
MH  - Chromatography, High Pressure Liquid
MH  - High-Throughput Screening Assays
MH  - Humans
MH  - Phenols/*urine
MH  - Solid Phase Extraction
MH  - Tandem Mass Spectrometry
OTO - NOTNLM
OT  - 96-well plate
OT  - endocrine disrupters
OT  - environmental phenols
OT  - solid phase extraction (SPE)
OT  - ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)
OT  - urine sample
EDAT- 2021/07/03 06:00
MHDA- 2021/07/28 06:00
CRDT- 2021/07/02 09:13
PHST- 2021/07/02 09:13 [entrez]
PHST- 2021/07/03 06:00 [pubmed]
PHST- 2021/07/28 06:00 [medline]
AID - 10.3724/SP.J.1123.2020.07021 [doi]
PST - ppublish
SO  - Se Pu. 2020 Dec 8;38(12):1456-1464. doi: 10.3724/SP.J.1123.2020.07021.