Article(id=1322945303485231115, tenantId=1146029695717560320, journalId=1283840372199657495, issueId=1322945277518295906, articleNumber=null, orderNo=null, doi=10.3724/SP.J.1123.2024.08005, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1723564800000, receivedDateStr=2024-08-14, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1793344339486, onlineDateStr=2026-10-30, pubDate=1749312000000, pubDateStr=2025-06-08, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1793344339486, onlineIssueDateStr=2026-10-30, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1793344339486, creator=13701087609, updateTime=1793344339486, updator=13701087609, issue=Issue{id=1322945277518295906, tenantId=1146029695717560320, journalId=1283840372199657495, year='2025', volume='43', issue='6', pageStart='559', pageEnd='709', issueExtLink='null', onlineDate='null', pubDate='1749312000000', pubDateStr='2025-06-08', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1793344333294, creator='13701087609', updateTime=1793345297848, updator='13701087609', preIssue=null, nextIssue=null, articleTotal=null, ext={EN=IssueExt(id=1322949323251654982, tenantId=1146029695717560320, journalId=1283840372199657495, issueId=1322945277518295906, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1322949323251654983, tenantId=1146029695717560320, journalId=1283840372199657495, issueId=1322945277518295906, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null, downloadFileDto=null}, startPage=659, endPage=669, ext={EN=ArticleExt(id=1322945303682363404, articleId=1322945303485231115, tenantId=1146029695717560320, journalId=1283840372199657495, language=EN, title=Analysis of four brominated flame retardants in mineral water and instant-noodle-bowl samples by magnetic solid-phase extraction coupled with liquid chromatography using magnetic carbon aerogel as adsorbent, columnId=1284557502633185292, journalTitle=Chinese Journal of Chromatography, columnName=Articles, runingTitle=null, highlight=null, articleAbstract=
Brominated flame retardants (BFRs) are widely used as organic flame retardants in plastic products, with most exhibiting strong biological toxicity as well as physical and chemical stability. BFRs inevitably remain in foods consumed on a daily basis through indirect or direct contact, thereby threatening human health. Therefore, establishing a fast and effective method for detecting and analyzing BFRs is imperative. Magnetic solid-phase extraction (MSPE) has been widely used in trace-analysis applications owing to advantages that include operational simplicity and rapid magnetic separability. The key to MSPE lies in the design and preparation of efficient magnetic adsorbents. In this study, a magnetic carbon aerogel (MCA) was prepared using a sol-gel method in combination with calcination. MCA was used as a magnetic solid-phase extractant to establish a new method for the analysis of four BFRs in mineral water and instant-noodle-bowl samples in combination with high performance liquid chromatography. Fourier-transform infrared (FT-IR) spectroscopy revealed peaks at 3 454, 1 590, 757, 1 349, 1 654, and 1 076 cm-1 that are ascribable to -NH2, -CH, triazine-ring, C-N, C=N, and C-O-C vibrations, respectively. Brunauer-Emmett-Teller (BET) analysis revealed values of 192.16 m2/g, 0.34 cm3/g, and 7.12 nm for the surface area, pore volume and pore size of the MCA, respectively. X-ray diffractometry (XRD) revealed a characteristic peak at 2θ=34.90° that corresponds to the (110) crystal plane of Fe2O3, and peaks at 2θ values of 44.72°, 65.01° and 82.42° that are ascribable to the (110), (200), and (211) crystal planes of CoFe/Co3Fe7. Vibrating sample magnetometry showed that the MCA is highly magnetic (35 emu/g), which contributes to fast magnetic solid-liquid separation. The MCA was characterized by transmission electron microscopy (TEM), which revealed a transparent gauze-like structure with nanometer-sized squares and circular particles evenly distributed between them. High-resolution TEM (HRTEM) showed that the square particles exhibit a 0.191 nm stripe spacing that belongs to the (311) crystal plane of Fe2O3, while the 0.245 nm stripe spacing observed for the circular particles corresponds to the (110) crystal plane of the CoFe alloy, in good agreement with the XRD results. X-ray photoelectron spectroscopy (XPS) revealed the presence of Co 2p, Fe 2p, O 1s, N 1s, and C 1s peaks. Taken together, these results show that the MCA, which contains various functional groups, had been successfully prepared. Factors that affect MSPE, such as solution pH, amount of material, adsorption time, the concentration and volume of the elution solvent, and sample volume, were investigated using the static adsorption method. BFR adsorption by the MCA was observed to increase with time, with equilibrium eventually reached. Tetrabromobisphenol A (TBBPA) reached adsorption equilibrium at 1 h with an adsorption rate close to 100%, whereas 3-bromobiphenyl (PBB-2), 4,4′-dibromobiphenyl (PBB-15), and 2,2′,4,4′-tetrabromodiphenyl ether (BDE-47) reached adsorption equilibria at 2 h. BDE-47 exhibited an adsorption rate close to 80% when 20 mg/L MCA was used, whereas the remaining three BFRs exhibited values close to 100%. Absorption by the MCA initially exhibited a constant trend with increasing sample volume but began to decline as the sample volume exceeded 100 mL. BFR adsorption by the MCA was found to be almost pH-independent, which indicates that the MCA is stable over a wide pH range. In addition, the analytes were effectively eluted in 30 min using 5 mL of acetonitrile. Based on the results presented above, the optimal adsorption and desorption conditions are: 20 mg/L of adsorbent, a sample volume of 100 mL, an adsorption time of 2 h without pH adjustment, 5 mL of acetonitrile as the eluent, and desorption time of 30 min. TBBPA, PBB-2, and PBB-15 exhibited limits of detection (LODs, S/N≥3) of 0.005 mg/L each under the optimal conditions, while BDE-47 exhibited a value of 0.010 mg/L, with corresponding RSDs of 7.35%, 5.12%, 3.66%, and 5.58% (n=5, C=0.02 mg/L), respectively, and actual enrichment times of 50, 40, 51, and 61 min, respectively. The developed method was used to determine four BFRs in mineral water and instant-noodle-bowl samples, with satisfactory recoveries obtained, thereby providing a new fast and sensitive method for the analysis of brominated flame retardants.
, authors=Qinrong NIE, Ming NI, Jiangyan XU, Ying SHI
*, Hongmei JIANG
*, authorsList=Qinrong NIE, Ming NI, Jiangyan XU, Ying SHI, Hongmei JIANG, authorCompany=null, correspAuthors=Ying SHI, Hongmei JIANG, authorNote=null, correspAuthorsNote=null, copyrightStatement=
This is an open access article distributed under the terms of the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original author and source are credited., copyrightOwner=null, extLink=null, articleAbsUrl=null, sourceXml=null, magXml=null, pdfUrl=null, pdf=null, pdfFileSize=null, pdfExtLink=null, richHtmlUrl=null, mobilePdfUrl=null, reviewReport=null, pdfFirstPage=null, abstractGraph=null, abstractGraphContent=null, abstractVideo=null, citation=null, cebUrl=null, magXmlContent=null, mapNumber=null, fund=null), CN=ArticleExt(id=1322945305729183775, articleId=1322945303485231115, tenantId=1146029695717560320, journalId=1283840372199657495, language=CN, title=磁性碳凝胶磁固相萃取与液相色谱联用分析矿泉水和泡面碗中4种溴代阻燃剂, columnId=1284557502792568846, journalTitle=色谱, columnName=研究论文, runingTitle=null, highlight=null, articleAbstract=
作为塑料制品中应用极广的有机阻燃剂,溴代阻燃剂大多具有较强的生物毒性和稳定的理化性质,通过间接或直接与食品接触,不可避免地残留在日常食物中,为人类健康带来潜在危害。因此,迫切需要建立一种快捷有效的溴代阻燃剂分析方法。磁固相萃取法因具有操作简单、可快速磁分离等优点,在痕量分析中得到了广泛的应用,该方法的关键在于高效磁性吸附剂的研制。本文提出以溶胶凝胶法结合煅烧法制备磁性碳凝胶,并以其为磁固相萃取材料,建立了磁固相萃取与高效液相色谱联用分析矿泉水和泡面碗中4种溴代阻燃剂的新方法。采用傅里叶变换红外光谱、X-射线衍射以及透射电镜等技术对材料的结构和组成进行表征,证实了磁性碳凝胶的成功制备。对影响磁固相萃取的因素如溶液pH值、材料用量、吸附时间、洗脱溶剂的浓度与体积和样品体积进行了详细考察,在最优条件下,本方法对四溴双酚A、3-溴联苯、4,4′-二溴联苯和四溴联苯醚的检出限(S/N≥3)分别为0.005、0.005、0.005和0.010 mg/L;RSD分别为7.35%、5.12%、3.66%和5.58%(n=5,C=0.02 mg/L);实际富集倍数分别为50、40、51和61倍。最后将所提出的方法应用于农夫山泉水样和塑料泡面碗中4种溴代阻燃剂的测定,获得了满意的加标回收结果,为溴代阻燃剂的分析提供了一种快捷、灵敏的新方法。
, authors=聂沁榕, 倪铭, 徐江艳, 施瑛
*, 蒋红梅
*, authorsList=聂沁榕, 倪铭, 徐江艳, 施瑛, 蒋红梅, authorCompany=null, correspAuthors=施瑛, 蒋红梅, authorNote=null, correspAuthorsNote=
, copyrightStatement=Copyright © 2025 Editorial office of Chinese Journal of Chromatography
本文是开放获取文章,遵循CC BY 4.0协议
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Chemical structure formulas of four brominated flame retardants (BFRs)TBBPA: tetrabromobisphenol A; PBB-2: 3-bromobiphenyl; PBB-15: 4,4′-dibromobiphenyl; BDE-47: 2,2′,4,4′-tetrabromodiphenyl ether.
, figureFileSmall=l2QsIDXNUbsqkt+fnn7+uA==, figureFileBig=+sEtGpSOy+oxUxi3o0T0cQ==, tableContent=null), ArticleFig(id=1322945310208700489, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322945303485231115, language=CN, label=图1, caption=
4种溴代阻燃剂的化学结构式, figureFileSmall=l2QsIDXNUbsqkt+fnn7+uA==, figureFileBig=+sEtGpSOy+oxUxi3o0T0cQ==, tableContent=null), ArticleFig(id=1322945310435192906, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322945303485231115, language=EN, label=Fig. 2, caption=
Flow diagram of magnetic solid-phase extraction (MSPE), figureFileSmall=bkx91OV3/TKaz6PbehV1oQ==, figureFileBig=jY1fqyZvw3jyLbGxSTNXBA==, tableContent=null), ArticleFig(id=1322945310506496075, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322945303485231115, language=CN, label=图2, caption=
磁固相萃取流程图, figureFileSmall=bkx91OV3/TKaz6PbehV1oQ==, figureFileBig=jY1fqyZvw3jyLbGxSTNXBA==, tableContent=null), ArticleFig(id=1322945311756398668, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322945303485231115, language=EN, label=Fig. 3, caption=
FT-IR spectrum of magnetic carbon aerogel (MCA), figureFileSmall=EttrPCGH0IeC/kjYVUaccQ==, figureFileBig=vi2cJdEckuqDyWo0EEvLPA==, tableContent=null), ArticleFig(id=1322945311848673357, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322945303485231115, language=CN, label=图3, caption=
磁性复合材料MCA的红外图, figureFileSmall=EttrPCGH0IeC/kjYVUaccQ==, figureFileBig=vi2cJdEckuqDyWo0EEvLPA==, tableContent=null), ArticleFig(id=1322945311974502478, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322945303485231115, language=EN, label=Fig. 4, caption=
N2 adsorption desorption isotherms of MCA, figureFileSmall=oJ84XI9VMcrUEwDV35IRaA==, figureFileBig=9KkxQ6zOluHX709tqdayCw==, tableContent=null), ArticleFig(id=1322945312133886031, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322945303485231115, language=CN, label=图4, caption=
复合材料MCA的氮气吸附脱附等温线, figureFileSmall=oJ84XI9VMcrUEwDV35IRaA==, figureFileBig=9KkxQ6zOluHX709tqdayCw==, tableContent=null), ArticleFig(id=1322945312226160721, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322945303485231115, language=EN, label=Fig. 5, caption=
XRD spectra of MCA, figureFileSmall=dCTOVMNmY/ij46DqkzNRcg==, figureFileBig=uIGXbbXSvN/+X18yWqMFXg==, tableContent=null), ArticleFig(id=1322945312284880978, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322945303485231115, language=CN, label=图5, caption=
复合材料MCA的XRD图, figureFileSmall=dCTOVMNmY/ij46DqkzNRcg==, figureFileBig=uIGXbbXSvN/+X18yWqMFXg==, tableContent=null), ArticleFig(id=1322945312372961363, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322945303485231115, language=EN, label=Fig. 6, caption=
Magnetic hysteresis loops of MCA, figureFileSmall=ax3EZcsPvSx0rVPjI95a3w==, figureFileBig=p+0zzJkgbNkG0wbwpqd2Zw==, tableContent=null), ArticleFig(id=1322945312444264532, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322945303485231115, language=CN, label=图6, caption=
复合材料MCA的磁滞曲线, figureFileSmall=ax3EZcsPvSx0rVPjI95a3w==, figureFileBig=p+0zzJkgbNkG0wbwpqd2Zw==, tableContent=null), ArticleFig(id=1322945312553316437, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322945303485231115, language=EN, label=Fig. 7, caption=
(a) Transmission electron microscope (TEM) image and (b, c) high resolution TEM images of MCA, figureFileSmall=qlIFZ/6pNFd95tuAlY8NVw==, figureFileBig=5Rv6bLsuo8hyPN+ND0og8g==, tableContent=null), ArticleFig(id=1322945312653979734, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322945303485231115, language=CN, label=图7, caption=
MCA的(a)透射电镜图谱和(b,c)高分辨透射电镜图谱, figureFileSmall=qlIFZ/6pNFd95tuAlY8NVw==, figureFileBig=5Rv6bLsuo8hyPN+ND0og8g==, tableContent=null), ArticleFig(id=1322945312750448727, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322945303485231115, language=EN, label=Fig. 8, caption=
XPS scan of MCA (a) and XPS separate scan of (b) Co 2p, (c) Fe 2p, (d) C 1s, (e) N 1s and (f) O 1s in MCA, figureFileSmall=VBRvT1nrNob59M0jCxkbYw==, figureFileBig=xEq1SQVJ8U0ys+dp2fEulA==, tableContent=null), ArticleFig(id=1322945312976941144, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322945303485231115, language=CN, label=图8, caption=
MCA的(a)XPS总谱、(b) Co 2p, (c) Fe 2p, (d) C 1s, (e) N 1s和(f) O 1s的XPS分谱图, figureFileSmall=VBRvT1nrNob59M0jCxkbYw==, figureFileBig=xEq1SQVJ8U0ys+dp2fEulA==, tableContent=null), ArticleFig(id=1322945313085993049, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322945303485231115, language=EN, label=Fig. 9, caption=
Effects of (a) adsorption time, (b) MCA dosage, (c) sample volume, (d) pH of sample, (e) eluent type, (f) elution volume and (g) elution time on the recoveries of the four BFRs, figureFileSmall=4rzd+15/06ZS+bClSF9e0A==, figureFileBig=vLdEbdUQcN0cH4Yrm88Ihg==, tableContent=null), ArticleFig(id=1322945313174073434, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322945303485231115, language=CN, label=图9, caption=
(a)吸附时间、(b)材料用量、(c)样品体积、(d) 样品pH、(e)洗脱剂类型、(f)洗脱剂体积和(g)洗脱时间对4种溴代阻燃剂回收率的影响, figureFileSmall=4rzd+15/06ZS+bClSF9e0A==, figureFileBig=vLdEbdUQcN0cH4Yrm88Ihg==, tableContent=null), ArticleFig(id=1322945313241182299, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322945303485231115, language=EN, label=Table 1, caption=
Analytical performance of the proposed method
, figureFileSmall=null, figureFileBig=null, tableContent=
| Analyte | Liner equation after MSPE a | R2 | LOD/(mg/L) | LOQ/(mg/L) | RSD/%b | Enrichment factor |
|---|
| TBBPA | Y=2732719.5X+2694.1 | 0.9998 | 0.005 | 0.0165 | 7.35 | 50 |
| PBB-2 | Y=2456021.1X-8836.9 | 0.9987 | 0.005 | 0.0165 | 5.12 | 40 |
| PBB-15 | Y=2696181.3X+147.4 | 0.9995 | 0.005 | 0.0165 | 3.66 | 51 |
| BDE-47 | Y=3315494.0X-8380.1 | 0.9993 | 0.010 | 0.033 | 5.58 | 61 |
), ArticleFig(id=1322945313333456988, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322945303485231115, language=CN, label=表 1, caption=
方法的分析性能
, figureFileSmall=null, figureFileBig=null, tableContent=
| Analyte | Liner equation after MSPE a | R2 | LOD/(mg/L) | LOQ/(mg/L) | RSD/%b | Enrichment factor |
|---|
| TBBPA | Y=2732719.5X+2694.1 | 0.9998 | 0.005 | 0.0165 | 7.35 | 50 |
| PBB-2 | Y=2456021.1X-8836.9 | 0.9987 | 0.005 | 0.0165 | 5.12 | 40 |
| PBB-15 | Y=2696181.3X+147.4 | 0.9995 | 0.005 | 0.0165 | 3.66 | 51 |
| BDE-47 | Y=3315494.0X-8380.1 | 0.9993 | 0.010 | 0.033 | 5.58 | 61 |
), ArticleFig(id=1322945313459286109, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322945303485231115, language=EN, label=Table 2, caption=
Comparison of this method with the reported methods
, figureFileSmall=null, figureFileBig=null, tableContent=
| Analysis method | Adsorbent | Analytes | Samples | LOD/(μg/L) | Ref. |
|---|
| SPE-HPLC | Br-COF | polybrominated diphenyl ethers | food | 0.01-0.05 | [35] |
| MSPE-GC-MS | micro-nano-structured magnetite particles | tetrabromobisphenol A, hexabromocyclododecane | water | 130-350 | [36] |
| MSPE-HPLC | NiFe2O4@COF | brominated flame retardants | water | 0.03-1.9 | [37] |
| MSPE-HPLC | Fe3O4@COF | brominated flame retardants | water | 0.15-0.39 | [38] |
| MSPE-HPLC | MCA | brominated flame retardants | water, plastic bowl | 5-10 | this work |
), ArticleFig(id=1322945313564143710, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322945303485231115, language=CN, label=表 2, caption=
本方法与文献报道方法比较
, figureFileSmall=null, figureFileBig=null, tableContent=
| Analysis method | Adsorbent | Analytes | Samples | LOD/(μg/L) | Ref. |
|---|
| SPE-HPLC | Br-COF | polybrominated diphenyl ethers | food | 0.01-0.05 | [35] |
| MSPE-GC-MS | micro-nano-structured magnetite particles | tetrabromobisphenol A, hexabromocyclododecane | water | 130-350 | [36] |
| MSPE-HPLC | NiFe2O4@COF | brominated flame retardants | water | 0.03-1.9 | [37] |
| MSPE-HPLC | Fe3O4@COF | brominated flame retardants | water | 0.15-0.39 | [38] |
| MSPE-HPLC | MCA | brominated flame retardants | water, plastic bowl | 5-10 | this work |
), ArticleFig(id=1322945313631252575, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322945303485231115, language=EN, label=Table 3, caption=
Detection of the four BFRs in mineral water and instant-noodle-bowl (n=3)
, figureFileSmall=null, figureFileBig=null, tableContent=
| Analyte | Spiked level/(μg/L) | Mineral water | Instant-noodle-bowl |
|---|
| Found/(μg/L) | Recovery/% | RSD/% | Found/(μg/L) | Recovery/% | RSD/% |
|---|
| TBBPA | 0 | ND | / | / | ND | / | / |
| 10 | 9.51 | 95.07 | 0.69 | 8.34 | 83.45 | 10.55 |
| 20 | 23.36 | 116.80 | 6.20 | 22.79 | 113.94 | 6.61 |
| PBB-2 | 0 | ND | / | / | ND | / | / |
| 10 | 6.55 | 65.50 | 12.83 | 7.70 | 77.04 | 4.19 |
| 20 | 17.11 | 85.54 | 3.59 | 17.26 | 86.31 | 5.20 |
| PBB-15 | 0 | ND | / | / | ND | / | / |
| 10 | 11.58 | 115.79 | 3.45 | 9.82 | 98.23 | 5.83 |
| 20 | 22.43 | 112.16 | 3.43 | 21.97 | 109.87 | 6.86 |
| BDE-47 | 0 | ND | / | / | ND | / | / |
| 10 | 5.89 | 58.91 | 8.16 | 6.63 | 66.38 | 14.23 |
| 20 | 14.29 | 71.48 | 4.87 | 15.05 | 75.26 | 5.18 |
), ArticleFig(id=1322945313765470304, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322945303485231115, language=CN, label=表 3, caption=
矿泉水和泡面碗中4种溴代阻燃剂的测定(n=3)
, figureFileSmall=null, figureFileBig=null, tableContent=
| Analyte | Spiked level/(μg/L) | Mineral water | Instant-noodle-bowl |
|---|
| Found/(μg/L) | Recovery/% | RSD/% | Found/(μg/L) | Recovery/% | RSD/% |
|---|
| TBBPA | 0 | ND | / | / | ND | / | / |
| 10 | 9.51 | 95.07 | 0.69 | 8.34 | 83.45 | 10.55 |
| 20 | 23.36 | 116.80 | 6.20 | 22.79 | 113.94 | 6.61 |
| PBB-2 | 0 | ND | / | / | ND | / | / |
| 10 | 6.55 | 65.50 | 12.83 | 7.70 | 77.04 | 4.19 |
| 20 | 17.11 | 85.54 | 3.59 | 17.26 | 86.31 | 5.20 |
| PBB-15 | 0 | ND | / | / | ND | / | / |
| 10 | 11.58 | 115.79 | 3.45 | 9.82 | 98.23 | 5.83 |
| 20 | 22.43 | 112.16 | 3.43 | 21.97 | 109.87 | 6.86 |
| BDE-47 | 0 | ND | / | / | ND | / | / |
| 10 | 5.89 | 58.91 | 8.16 | 6.63 | 66.38 | 14.23 |
| 20 | 14.29 | 71.48 | 4.87 | 15.05 | 75.26 | 5.18 |
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