干旱区生态环境知识资源中心(Arid): Determination of eight environmental phenols in human urine samples by high-throughput solid-phase extraction-ultra-performance liquid chromatography-tandem mass spectrometry

Arid

DOI	10.3724/SP.J.1123.2020.07021
	Determination of eight environmental phenols in human urine samples by high-throughput solid-phase extraction-ultra-performance liquid chromatography-tandem mass spectrometry
	Lin Xiao; Qiu Tian; Zhang Xu; Hu Xiaojian; Yang Yanwei; Zhu Ying
通讯作者	Zhu, Y (corresponding author), Chinese Ctr Dis Control & Prevent, Natl Inst Environm Hlth, China CDC Key Lab Environm & Populat Hlth, Beijing 100021, Peoples R China.
来源期刊	CHINESE JOURNAL OF CHROMATOGRAPHY
ISSN	1000-8713
出版年	2020
卷号	38 期号:12 页码:1456-1464
英文摘要	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 mu m) 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, tetra-chlorobisphenol 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 mu g / L for bisphenol A and bis-phenol AF; 0. 05- 50 mu g / L for tetrachlorobisphenol A and bisphenol S; 0. 01- 50 mu g / L for bis-phenol F and tetrabromobisphenol A; 1. 00- 50 mu g / L for bisphenol B; and 5. 00- 200 mu g / L for triclosan. The correlation coefficients were all greater than 0. 999 5. At spiked levels of 2. 5, 5, and 25 mu g / 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 mu g / L, and the limits of quantitation ( LOQ) were 0. 007- 3. 63 mu g / 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 bis-phenol AF. Bisphenol A and bisphenol S showed the highest detection rates of 100% and 96. 9%, respectively. The detection rates of triclosan, tetrabromobisphenol A, tetrachlorobis-phenol 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 mu g / L( triclosan), 0. 69 mu g / L( bisphenol A), 0. 086 mu g / L ( bisphenol S), 0. 003 2 mu g / L ( tetrabromobisphenol A), 0. 000 50 mu g / L ( tetra-chlorobisphenol A), 0. 00 mu g / 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.
英文关键词	solid phase extraction (SPE) ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) environmental phenols endocrine disrupters urine sample 96-well plate
类型	Article
语种	中文
收录类别	ESCI
WOS记录号	WOS:000605716700013
WOS关键词	BISPHENOL-A ; HUMAN EXPOSURE ; TRICLOSAN ; BPA ; CHILDREN ; HEALTH ; ADULTS
WOS类目	Chemistry, Analytical
WOS研究方向	Chemistry
资源类型	期刊论文
条目标识符	http://119.78.100.177/qdio/handle/2XILL650/352532
作者单位	[Lin Xiao; Qiu Tian; Zhang Xu; Hu Xiaojian; Yang Yanwei; Zhu Ying] Chinese Ctr Dis Control & Prevent, Natl Inst Environm Hlth, China CDC Key Lab Environm & Populat Hlth, Beijing 100021, Peoples R China
推荐引用方式 GB/T 7714	Lin Xiao,Qiu Tian,Zhang Xu,et al. Determination of eight environmental phenols in human urine samples by high-throughput solid-phase extraction-ultra-performance liquid chromatography-tandem mass spectrometry[J],2020,38(12):1456-1464.
APA	Lin Xiao,Qiu Tian,Zhang Xu,Hu Xiaojian,Yang Yanwei,&Zhu Ying.(2020).Determination of eight environmental phenols in human urine samples by high-throughput solid-phase extraction-ultra-performance liquid chromatography-tandem mass spectrometry.CHINESE JOURNAL OF CHROMATOGRAPHY,38(12),1456-1464.
MLA	Lin Xiao,et al."Determination of eight environmental phenols in human urine samples by high-throughput solid-phase extraction-ultra-performance liquid chromatography-tandem mass spectrometry".CHINESE JOURNAL OF CHROMATOGRAPHY 38.12(2020):1456-1464.