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氢氧化四甲铵萃取后用电感耦合等离子体质谱法(ICPMS)测定人母乳中碘的优化方法的验证

Validation of an optimized method for the determination of iodine in human breast milk by inductively coupled plasma mass spectrometry (ICPMS) after tetramethylammonium hydroxide extraction.

作者信息

Huynh Dao, Zhou Shao Jia, Gibson Robert, Palmer Lyndon, Muhlhausler Beverly

机构信息

FOODplus Research Centre, School of Agriculture Food and Wine, The University of Adelaide, Adelaide 5064, South Australia, Australia.

FOODplus Research Centre, School of Agriculture Food and Wine, The University of Adelaide, Adelaide 5064, South Australia, Australia; Women's and Children's Health Research Institute, Women's and Children's Hospital, King William Road, North Adelaide 5006, South Australia, Australia.

出版信息

J Trace Elem Med Biol. 2015 Jan;29:75-82. doi: 10.1016/j.jtemb.2014.07.005. Epub 2014 Aug 1.

Abstract

In this study a novel method to determine iodine concentrations in human breast milk was developed and validated. The iodine was analyzed by inductively coupled plasma mass spectrometry (ICPMS) following tetramethylammonium hydroxide (TMAH) extraction at 90°C in disposable polypropylene tubes. While similar approaches have been used previously, this method adopted a shorter extraction time (1h vs. 3h) and used antimony (Sb) as the internal standard, which exhibited greater stability in breast milk and milk powder matrices compared to tellurium (Te). Method validation included: defining iodine linearity up to 200μgL(-1); confirming recovery of iodine from NIST 1549 milk powder. A recovery of 94-98% was also achieved for the NIST 1549 milk powder and human breast milk samples spiked with sodium iodide and thyroxine (T4) solutions. The method quantitation limit (MQL) for human breast milk was 1.6μgL(-1). The intra-assay and inter-assay coefficient of variation for the breast milk samples and NIST powder were <1% and <3.5%, respectively. NIST 1549 milk powder, human breast milk samples and calibration standards spiked with the internal standard were all stable for at least 2.5 months after extraction. The results of the validation process confirmed that this newly developed method provides greater accuracy and precision in the assessment of iodine concentrations in human breast milk than previous methods and therefore offers a more reliable approach for assessing iodine concentrations in human breast milk.

摘要

在本研究中,开发并验证了一种测定人乳中碘浓度的新方法。在一次性聚丙烯管中于90°C用氢氧化四甲铵(TMAH)萃取后,通过电感耦合等离子体质谱法(ICPMS)分析碘。虽然此前已使用过类似方法,但该方法采用了更短的萃取时间(1小时对比3小时),并使用锑(Sb)作为内标,与碲(Te)相比,锑在母乳和奶粉基质中表现出更高的稳定性。方法验证包括:确定碘在高达200μg/L(-1)范围内的线性;确认从NIST 1549奶粉中回收碘。对于添加了碘化钠和甲状腺素(T4)溶液的NIST 1549奶粉和人乳样品,回收率也达到了94 - 98%。人乳的方法定量限(MQL)为1.6μg/L(-1)。母乳样品和NIST奶粉的批内和批间变异系数分别<1%和<3.5%。添加了内标的NIST 1549奶粉、人乳样品和校准标准品在萃取后至少2.5个月内均保持稳定。验证过程的结果证实,这种新开发的方法在评估人乳中碘浓度方面比以前的方法具有更高的准确性和精密度,因此为评估人乳中碘浓度提供了一种更可靠的方法。

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