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二甲基甲醯胺生物偵測技術之引進探討

Characteristic Study of the Biological Monitoring of Occupational Exposure to Dimethlformamide

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摘要


二甲基甲醯安(DMF)是常用的有機溶劑,它能迅速穿透皮膚與黏膜而進入人體,它的毒性標的器官有肝臟及睪丸。美國ACGIH及德國DFG對暴露於DMF的生物偵測皆建議以氣相層析(GC/FID)分析尿中單甲基甲醯胺(NMF)之量為指標,目前它的暴露參考值ACGIH正準備由40mg/g肌酸酐降為20mg/g,德國的參考值則是15 mg/L尿。 人及大鼠暴露於DMF後,尿中排出的主要代謝物為DMF-OH,此代謝物不是很穩定,目前並無市售之標準品,它出現於GC圖譜的是其加熱後之裂解物NMF。因此DMF之生物偵測分析,是以兩份冷甲醇(含內標)來處理尿檢體、經離心後上GC分析,以NMF製備檢量線。 我譬的檢量線範圍為1~9μg/mL,內標是單甲基乙醯胺(NMA),所有的異日變異係數(%CV,加或不加連共10組)都≤10%,n=4,所有的%相對誤都≤±10%,回收率以斜率比表示,則有100.3±10.2%,n=4。偵測極限為0.056安欠2μL,即0.028μg/mL。濃度接近參考值之品管樣品(三種),其製備是以未經暴露之人尿稀釋經DMF暴露之鼠尿而得。儲存於-30˚C之穩定度是以品管栓品來探討,結果發現穩定度至少有38天。以此方法分析所得的39個下班前工人之檢體,發現四個檢體在NMF的滯留時間處有一小波峰,經外加法確認,只得一人有微量之NMF,0.289μg/mL(低於目前的檢量線)約相當於0.120μg/mL肌酸酐。本方法曾經部份經過不同分析員、不同實驗室、不同GC儀器、不同線性範圍之驗證,發現再現性佳,百分相對誤均小於±10%,只是有的儀器感度(GC/FID)較差,無法有效地分析≤4μg/mL之NMF。 [本研究承蒙行政院勞工安全衛生研究所(IOSH 85-A310)之資,謹此致謝]。

關鍵字

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並列摘要


Dimethylformamide (DMF) is an important industrial organic solvent. It is readily absorbed through mucosa and skin. DMF is hepatotoxic and may induce tumors in testis. To monitor workers’ exposure, both ACGIH of US and German DFG recommend a GC/FID analysis of urinary monmethyl-formamide (NMF). The recommended reference value is 15mg/L urine by the DFG and 40 mg/g creatinine by ACGIH. ACGIH is proposing to change it to 20 mg/g creatinine. NMF is the thermal decomposition product of DMF-OH, the major urinary metabolite, which is unstable and currently not available commercially. Our monitoring method differed from others in 2 aspects: (1) a brief centrifugation to remove particulates after the treatment with cold methanol and (2) analysis with an intemal standard, monomethylacetamide. The method established had (1) a linear range of 1~9 μg NMF/mL, (2)all interday %Cvs≤10%. (10sets of them, with and without media, n=4)(3) all% relative errors≤±10%,(4)a recovery of, as slope ratio, 100.3±10.2% (n=4), and (5) a detection limit of 0.028 μ g/mL. Three series of QC samples, with concentrations close to the reference values, were prepared by diluting the DMF-exposed rat urines with unexposed human urine. Sample stability was found to have 38 days at-30˚C. An operating SOP was written and used to evaluate 39 post-shift samples. Four of them sowed a small signal at the retention place of NMF. Standard addition method was used to confirm its identity. Only one of the 4 was truly NMF. Its concentration was estimated, by extrapolation, to be 0.29μg/mL. The method was quasi-verified without simultaneously analyzing a group of identical samples. We’ve found that (1) the method worked satisfactorily by various hands, (2) all interday %Cvs and all % relative errors were≤10%, and (3)some GC/FID can not effectively analyze samples of urinary NMF of ≤4μg/mL. (The financial support by the IOSH85-A310 of ROC is acknowledged.)

並列關鍵字

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被引用紀錄


黃偉銘(2015)。樟腦衍生之掌性β-胺基醇及β-胺基硫醇在催化不對稱加成反應之研究〔博士論文,國立清華大學〕。華藝線上圖書館。https://www.airitilibrary.com/Article/Detail?DocID=U0016-0312201510260329

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