超级微波消解ICP-OES法测定宠物饲料中硫含量及与总蛋白质相关性分析

doi:10.3964/j.issn.1000-0593(2025)02-0420-06

摘要
参考文献
相关文章 (15)

全文: PDF (2062 KB)
输出: BibTeX | EndNote (RIS)

摘要：建立了超级微波消解-电感耦合等离子体发射光谱法（ICP-OES）测定宠物饲料中硫含量的新方法。系统探究了超级微波消解条件对消解液中残留碳含量（RCC）和残留酸量（RA）的影响，以这两项指标为依据，有效评估了消解效果，建立了优化微波消解条件的新策略。系统性研究了五种不同价态的硫形态对硫元素测定的影响，发现低价态硫标准物质在酸性条件下制备时，硫元素发射强度显著增强，而高价态硫标准物质在三种条件（酸性、中性和碱性）下制备时，硫元素发射强度均较稳定，为配制介质和硫标准物质的选择提供了有益的指导。研究发现，超级微波消解系统所创造的高温高压环境以及消解试剂的强氧化性条件，能有效消除低价态硫在酸性前处理条件下的发射强度增强效应。采用酸性条件配制高价态硫（SO^2-₄）标准物质，并结合超级微波消解系统，能够实现宠物饲料中五种不同价态硫的准确测定。加标回收率为86.5％～108％，RSD值为1.69％～4.18％，检出限为6.2 mg·kg^-1，与国家标准方法相比，该方法具有灵敏度高、成本低、绿色环保、工作效率高的优点。研究发现宠物饲料中硫含量与总蛋白质含量之间存在极显著正相关性（相关系数=0.819，p＜0.01），可以为宠物饲料中总蛋白质含量的准确测定提供新思路和方向。

关键词：超级微波消解；超级微波消解-电感耦合等离子体发射光谱（ICP-OES）；宠物饲料；硫；总蛋白质；相关性

Abstract：A novel method for determining the sulfur content in pet feeds was established using a super microwave digestion system and inductively coupled plasma optical emission spectrometry (ICP-OES) in the study. For the first time, we systematically investigated the effects of super microwave digestion conditions on residual carbon content (RCC) and residual acid (RA) in the digestion solution. We evaluated the digestion effects effectively and developed a new strategy for optimizing microwave digestion conditions based on these indicators. Furthermore, we thoroughly examined the influence of five different sulfur species on sulfur determination. We found that the emission intensity of sulfur was significantly enhanced by preparing low-valent sulfur standard substances under acidic conditions. However, when high-valent sulfur standard substances were prepared under acidic, neutral, or alkaline conditions, the emission intensity of sulfur remained relatively stable. This provided useful guidance for selecting preparation media and sulfur standard substances. Additionally, our research revealed that the super microwave digestion system effectively eliminated the enhanced emission intensity effect of low-valent sulfur under acidic conditions. In summary, the accurate determination of five different valence states of sulfur in pet feeds can be achieved by preparing high valence sulfate (SO^2-₄) standard substance under acidic conditions using the super microwave digestion system. The recoveries ranged from 86.5%~108%, and the RSD was between 1.69% and 4.18%. The detection limit was 6.2 mg·kg^-1. Compared with the national standard method, this method had high sensitivity, low cost, environmental friendliness, and high work efficiency. Furthermore, a significant positive correlation was observed between sulfur and total protein content in pet feeds (correlation coefficient=0.819, p<0.01). This conclusion can provide new ideas and directions for accurately determining pet feed protein content.

Key words：Super microwave digestion; ICP-OES; Pet feeds; Sulfur; Total protein; Correlation

收稿日期: 2024-01-25 修订日期: 2024-04-29

中图分类号:

O657.3

基金资助: 深圳市可持续发展专项（KCXFZ20230731092859013），深圳市自然科学基金项目（JCYJ20210324141801003），2023年度广东省质监局科技项目(2023CS05)资助

通讯作者: 陈晓燕，郑彦婕 E-mail: 634403201@qq.com；smq1234567@163.com

作者简介: 陈树娣，女，1982年生，深圳市计量质量检测研究院高级工程师 e-mail: 164793222@qq.com

引用本文:

陈树娣，李锦才，陈晓燕，李胜，张世伟，郑彦婕. 超级微波消解ICP-OES法测定宠物饲料中硫含量及与总蛋白质相关性分析[J]. 光谱学与光谱分析, 2025, 45(02): 420-425.
CHEN Shu-di, LI Jin-cai, CHEN Xiao-yan, LI Sheng, ZHANG Shi-wei, ZHENG Yan-jie. Determination of S and the Correlation With Total Protein in Pet Feeds by Super Microwave Digestion ICP-OES. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2025, 45(02): 420-425.

链接本文:

https://www.gpxygpfx.com/CN/10.3964/j.issn.1000-0593(2025)02-0420-06 或 https://www.gpxygpfx.com/CN/Y2025/V45/I02/420

[1] LI Xiu-hua（李秀花）. Chinese Qinghai Journal of Animal and Veterinary Sciences（青海畜牧兽医杂志），2008，38（1）：14.
[2] National Stndards of the People's Republic of China（中华人民共和国国家标准）. GB/T17776—2016 Determination of Sulfur in Feedstuff-Magnesium Nitrate Method(GB/T17776—2016 饲料中硫的测定硝酸镁法). Beijing：Standars Press of China(北京：中国标准出版社)，2016.
[3] ZHANG Zong-xiang，ZHU Yu-fang（张宗祥，朱宇芳）. Fujian Analysis & Testing（福建分析测试），2007，16(3)：65.
[4] SUN Hai-tao，ZHANG Ying（孙海涛，张颖）. Environmental Monitoring and Forewarning（环境监控与预警），2017，9(4)：35.
[5] ZHAO Dong-rui，ZHANG Li-mo，ZHANG Feng-guo，et al（赵东瑞，张丽末，张锋国，等）. Food Science（食品科学），2016，37(22)：99.
[6] CUI Yu-hong，FAN Kai-zhen，GUO Jing-wen，et al（崔宇宏，樊开珍，郭景文，等）. Chin J Phamn Anal（药物分析杂志），2012，31(1)：123.
[7] Dalen G V. X-Ray Spectrometry，1998，27(1)：26.
[8] ZHANG Qi，LIU Lin-juan（张琪，刘琳娟）. Chemical Analysis and Meterage（化学分析计量），2007，16(2)：40.
[9] Marrocos V C P，Gonçalves R A，Lepri F G，et al. SpectrochimicaActa Part B: Atomic Spectroscopy，2020，174：106008.
[10] ZHAO Xiao-xue，WANG Jian-bo，WANG Long-fei，et al（赵小学，王建波，王龙飞，等）. Environmental Monitoring in China（中国环境监测），2022，38(2)：164.
[11] ZHAO Liu-hong，LAN Chang-bo（赵柳红，蓝长波）. Journal of Food Safety and Quality（食品安全质量检测学报），2019，10(20)：6.
[12] LU Li，LIU Er-long，ZHAN Ye-tian，et al（卢丽，刘二龙，詹业添，等）. Journal of Food Safety and Quality（食品安全质量检测学报），2018，9(3)：564.
[13] Yang J，Conver T S，Koropchak J A. Anal. Chem.，1996，68：4064.
[14] Langlois B，Dautheribes J L，MermetJ. M. J. Anal. At. Spectrom.，2003，18：76.
[15] Montiel J，Grinday G，Gras L，et al. Spectrochimica Acta Part B，2013，81：36.
[16] National Stndards of the People's Republic of China（中华人民共和国国家标准）. GB/T6432—2018 Determination of Crude Protein in Feeds-Kjeldahl Method(GB/T6432—2018 饲料中粗蛋白的测定凯氏定氮法). Beijing：Standars Press of China（北京：中国标准出版杜），2018.