Article(id=1217529307971376028, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1217529305693864468, articleNumber=null, orderNo=null, doi=10.19812/j.cnki.jfsq11-5956/ts.20250103002, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1735833600000, receivedDateStr=2025-01-03, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1768211207620, onlineDateStr=2026-01-12, pubDate=1752508800000, pubDateStr=2025-07-15, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1768211207620, onlineIssueDateStr=2026-01-12, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1768211207620, creator=13701087609, updateTime=1768211207620, updator=13701087609, issue=Issue{id=1217529305693864468, tenantId=1146029695717560320, journalId=1149652044408987649, year='2025', volume='16', issue='13', pageStart='1', pageEnd='320', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1768211207077, creator=13701087609, updateTime=1768212057891, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1217532874337730593, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1217529305693864468, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1217532874337730594, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1217529305693864468, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=189, endPage=194, ext={EN=ArticleExt(id=1217529309519074212, articleId=1217529307971376028, tenantId=1146029695717560320, journalId=1149652044408987649, language=EN, title=Exploration of key issues and method optimization of GB 5009.3—2016 National food safety standard-Determination of moisture in foods, columnId=1151895321388347923, journalTitle=Journal of Food Safety & Quality, columnName=Food Analysis and Detection, runingTitle=null, highlight=null, articleAbstract=

Objective To analyze the key factors affecting constant weight in the direct drying method and to optimize the experimental conditions for vacuum drying, distillation, and Karl Fischer methods as specified in the GB 5009.3—2016 National food safety standard-Determination of moisture in foods. Methods The determination of moisture content in samples was conducted according to GB 5009.3—2016. The study altered experimental conditions to explore key factors affecting constant weight in the direct drying method, optimized conditions for vacuum drying by adjusting vacuum pressure, and compared the effects of different reagents (xylene, Karl Fischer reagent) on detection results. Results In the direct drying method, sample temperature, cooling time in the desiccator and the degree of sample pulverization were identified as key factors affecting constant weight. For vacuum drying method, increasing the vacuum to -0.1 MPa and adding an effective desiccant to the drying box could rapidly evaporate moisture from the sample, improving detection efficiency. In the distillation method, the preparation and purification of analytical-grade toluene or xylene could be omitted. The Karl Fischer method could use a low-toxicity, pyridine-free Karl Fischer reagent. Conclusion The 4 detection methods in this standard are optimized separately to solve problems such as difficulty in achieving constant weight after repeated drying and the use of toxic and harmful reagents. The rationalization suggestions provide in this study have increased the operability of the standard and improved the testing efficiency of the laboratory.

, correspAuthors=Sheng WEN, authorNote=null, correspAuthorsNote=null, copyrightStatement=null, 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, authorCompany=null, fund=null, authors=null, authorsList=Fang KONG, Yong-Gang LI, Xiao-Hong LIU, Xiao-Tian ZHANG, Guo-Qiang LI, Chao-Jun YUAN, Li HOU, Sheng WEN), CN=ArticleExt(id=1217529311008052181, articleId=1217529307971376028, tenantId=1146029695717560320, journalId=1149652044408987649, language=CN, title=GB 5009.3—2016《食品安全国家标准 食品中水分的测定》的关键问题探讨及方法优化, columnId=1151895321958773274, journalTitle=食品安全质量检测学报, columnName=食品分析与检测, runingTitle=null, highlight=null, articleAbstract=

目的 分析GB 5009.3—2016《食品安全国家标准 食品中水分的测定》中直接干燥法操作步骤中影响恒重的关键因素, 并优化减压干燥法、蒸馏法和卡尔·费休法的试验条件。方法 样品中水分含量测定参照GB 5009.3—2016进行。同时, 改变实验条件探讨直接干燥法中影响恒重的关键因素; 改变真空压力优化减压干燥法的条件; 比较不同的试剂(二甲苯试剂、卡尔·费休试剂)对检测结果的影响。结果 直接干燥法中, 样品温度、干燥器内冷却时间和样品粉碎程度等3个方面是影响恒重的关键因素; 减压干燥法中, 真空度提高到-0.1 MPa, 并在干燥箱内加入有效干燥剂, 可快速挥发出样品中的水分, 提高检测效率; 蒸馏法中分析纯甲苯或二甲苯试剂的制备提纯可删除; 卡尔·费休法可采用低毒性的无吡啶卡尔·费休试剂。结论 对该标准中的4个检测方法分别进行优化, 解决了反复烘干难以达到恒重、使用有毒有害试剂等问题。本研究提供的合理化建议, 增加了该标准的可操作性, 提高了实验室的检测效率。

, correspAuthors=闻胜, authorNote=null, correspAuthorsNote=
*闻胜(1977—), 男, 博士, 研究员, 主要研究方向为食品安全。E-mail:
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孔芳(1987—), 女, 硕士, 主管技师, 主要研究方向为食品安全检测。E-mail:

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Metrology & Measurement Technique, 2016, 43(10): 34-35., articleTitle=The Influence of environment temperature on the accuracy of high precision electronic balance, refAbstract=null), Reference(id=1217901271890186490, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529307971376028, doi=null, pmid=null, pmcid=null, year=2011, volume=25, issue=3, pageStart=41, pageEnd=42, url=null, language=null, rfNumber=[29], rfOrder=53, authorNames=逯亚飞, journalName=现代面粉工业, refType=null, unstructuredReference=逯亚飞. 对食品水分测定时冷却时间的探讨[J]. 现代面粉工业, 2011, 25(3): 41-42., articleTitle=对食品水分测定时冷却时间的探讨, refAbstract=null), Reference(id=1217901271982461181, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529307971376028, doi=null, pmid=null, pmcid=null, year=2011, volume=25, issue=3, pageStart=41, pageEnd=42, url=null, language=null, rfNumber=[29], rfOrder=54, authorNames=LV YF, journalName=Modern Flour Milling Industry, refType=null, unstructuredReference=LV YF. 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Modern Flour Milling Industry, 2011, 25(3): 41-42., articleTitle=Discussion on the cooling time in the determination of moisture content in foods, refAbstract=null), Reference(id=1217901272074735870, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529307971376028, doi=null, pmid=null, pmcid=null, year=2021, volume=50, issue=1, pageStart=48, pageEnd=52, url=null, language=null, rfNumber=[30], rfOrder=55, authorNames=徐宗季, 王平东, 袁华山, journalName=粮食储藏, refType=null, unstructuredReference=徐宗季, 王平东, 袁华山, 等. 不同水分磨的粉碎细度对粮食水分含量的影响[J]. 粮食储藏, 2021, 50(1): 48-52., articleTitle=不同水分磨的粉碎细度对粮食水分含量的影响, refAbstract=null), Reference(id=1217901272171204866, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529307971376028, doi=null, pmid=null, pmcid=null, year=2021, volume=50, issue=1, pageStart=48, pageEnd=52, url=null, language=null, rfNumber=[30], rfOrder=56, authorNames=XU ZJ, WANG PD, YUAN HS, journalName=Grain Storage, refType=null, unstructuredReference=XU ZJ, WANG PD, YUAN HS, et al. Effect of grinding fineness of different moisture mills on grain moisture content[J]. 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Moisture content measured under different pressures

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样品基质 直接干燥法/(g/100 g) 减压干燥法(65 ℃)
50 kPa -0.1 MPa -0.1 MPa+干燥剂
水分含量
/(g/100 g)
减压/直接干燥法/% 水分含量
/(g/100 g)
减压/直接干燥法/% 水分含量
/(g/100 g)
减压/直接干燥法/%
奶粉 4.87 3.86 79.3 4.31 88.5 4.61 94.7
玉米粉 11.90 9.48 79.7 10.60 89.1 11.40 95.8
马铃薯淀粉 17.90 15.00 83.8 16.60 92.7 17.10 95.5
), ArticleFig(id=1217901262826296269, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529307971376028, language=CN, label=表1, caption=

不同压力下测得的水分含量

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样品基质 直接干燥法/(g/100 g) 减压干燥法(65 ℃)
50 kPa -0.1 MPa -0.1 MPa+干燥剂
水分含量
/(g/100 g)
减压/直接干燥法/% 水分含量
/(g/100 g)
减压/直接干燥法/% 水分含量
/(g/100 g)
减压/直接干燥法/%
奶粉 4.87 3.86 79.3 4.31 88.5 4.61 94.7
玉米粉 11.90 9.48 79.7 10.60 89.1 11.40 95.8
马铃薯淀粉 17.90 15.00 83.8 16.60 92.7 17.10 95.5
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Effects of purified and non-purified analytical-grade xylene on the moisture content in the sample

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编号 样品名称 蒸馏法/(g/100 g) 相对偏差/%
未提纯 提纯
1 蜜枣 11.80 11.70 -0.85
2 山楂饴 18.00 18.10 0.55
3 果丹皮 15.40 15.30 -0.65
4 话梅 39.40 39.30 -0.25
5 葡萄干 14.50 14.50 0
6 山楂片 8.19 8.08 -1.36
7 果蔬脆 4.51 4.48 -0.67
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提纯和未提纯的分析纯二甲苯对样品中水分含量的影响

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编号 样品名称 蒸馏法/(g/100 g) 相对偏差/%
未提纯 提纯
1 蜜枣 11.80 11.70 -0.85
2 山楂饴 18.00 18.10 0.55
3 果丹皮 15.40 15.30 -0.65
4 话梅 39.40 39.30 -0.25
5 葡萄干 14.50 14.50 0
6 山楂片 8.19 8.08 -1.36
7 果蔬脆 4.51 4.48 -0.67
), ArticleFig(id=1217901263195395039, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529307971376028, language=EN, label=Table 3, caption=

Effects of Karl Fischer reagent with and without pyridine on the moisture content in the sample (n=6)

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样品基质 卡尔·费休试剂 水分含量/(g/100 g) 平均值
/(g/100 g)
RSDs
/%
P
1 2 3 4 5 6
食用调和油 无吡啶 0.086 0.089 0.089 0.089 0.089 0.089 0.089 1.38 0.66
含吡啶 0.089 0.088 0.088 0.088 0.087 0.089 0.088 0.85
猪油 无吡啶 0.044 0.045 0.044 0.044 0.045 0.045 0.045 1.23 0.36
含吡啶 0.045 0.046 0.044 0.045 0.044 0.045 0.045 1.68
无水奶油 无吡啶 0.041 0.042 0.042 0.041 0.041 0.042 0.042 1.32 0.61
含吡啶 0.040 0.042 0.041 0.042 0.041 0.042 0.041 1.98
), ArticleFig(id=1217901263329612772, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217529307971376028, language=CN, label=表3, caption=

含吡啶和无吡啶卡尔·费休试剂对样品中水分含量的影响(n=6)

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样品基质 卡尔·费休试剂 水分含量/(g/100 g) 平均值
/(g/100 g)
RSDs
/%
P
1 2 3 4 5 6
食用调和油 无吡啶 0.086 0.089 0.089 0.089 0.089 0.089 0.089 1.38 0.66
含吡啶 0.089 0.088 0.088 0.088 0.087 0.089 0.088 0.85
猪油 无吡啶 0.044 0.045 0.044 0.044 0.045 0.045 0.045 1.23 0.36
含吡啶 0.045 0.046 0.044 0.045 0.044 0.045 0.045 1.68
无水奶油 无吡啶 0.041 0.042 0.042 0.041 0.041 0.042 0.042 1.32 0.61
含吡啶 0.040 0.042 0.041 0.042 0.041 0.042 0.041 1.98
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GB 5009.3—2016《食品安全国家标准 食品中水分的测定》的关键问题探讨及方法优化
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孔芳 1 , 李永刚 1 , 刘小红 1 , 张晓甜 1 , 李国强 2 , 袁超君 2 , 侯力 2 , 闻胜 1, *
食品安全质量检测学报 | 食品分析与检测 2025,16(13): 189-194
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食品安全质量检测学报 | 食品分析与检测 2025, 16(13): 189-194
GB 5009.3—2016《食品安全国家标准 食品中水分的测定》的关键问题探讨及方法优化
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孔芳1 , 李永刚1, 刘小红1, 张晓甜1, 李国强2, 袁超君2, 侯力2, 闻胜1, *
作者信息
  • 1 湖北省疾病预防控制中心, 国家卫生健康委员会食品安全风险评估与标准研制特色实验室, 武汉 430079
  • 2 应城市疾病预防控制中心, 应城 432400
  • 孔芳(1987—), 女, 硕士, 主管技师, 主要研究方向为食品安全检测。E-mail:

通讯作者:

*闻胜(1977—), 男, 博士, 研究员, 主要研究方向为食品安全。E-mail:
Exploration of key issues and method optimization of GB 5009.3—2016 National food safety standard-Determination of moisture in foods
Fang KONG1 , Yong-Gang LI1, Xiao-Hong LIU1, Xiao-Tian ZHANG1, Guo-Qiang LI2, Chao-Jun YUAN2, Li HOU2, Sheng WEN1, *
Affiliations
  • 1 Hubei Provincial Center for Disease Control and Prevention, National Health Commission Specialty Laboratory of Food Safety Risk Assessment and Standard Development, Wuhan 430079, China
  • 2 Yingcheng City Center for Disease Control and Prevention, Yingcheng 432400, China
出版时间: 2025-07-15 doi: 10.19812/j.cnki.jfsq11-5956/ts.20250103002
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目的 分析GB 5009.3—2016《食品安全国家标准 食品中水分的测定》中直接干燥法操作步骤中影响恒重的关键因素, 并优化减压干燥法、蒸馏法和卡尔·费休法的试验条件。方法 样品中水分含量测定参照GB 5009.3—2016进行。同时, 改变实验条件探讨直接干燥法中影响恒重的关键因素; 改变真空压力优化减压干燥法的条件; 比较不同的试剂(二甲苯试剂、卡尔·费休试剂)对检测结果的影响。结果 直接干燥法中, 样品温度、干燥器内冷却时间和样品粉碎程度等3个方面是影响恒重的关键因素; 减压干燥法中, 真空度提高到-0.1 MPa, 并在干燥箱内加入有效干燥剂, 可快速挥发出样品中的水分, 提高检测效率; 蒸馏法中分析纯甲苯或二甲苯试剂的制备提纯可删除; 卡尔·费休法可采用低毒性的无吡啶卡尔·费休试剂。结论 对该标准中的4个检测方法分别进行优化, 解决了反复烘干难以达到恒重、使用有毒有害试剂等问题。本研究提供的合理化建议, 增加了该标准的可操作性, 提高了实验室的检测效率。

水分测定  /  国家标准  /  关键问题

Objective To analyze the key factors affecting constant weight in the direct drying method and to optimize the experimental conditions for vacuum drying, distillation, and Karl Fischer methods as specified in the GB 5009.3—2016 National food safety standard-Determination of moisture in foods. Methods The determination of moisture content in samples was conducted according to GB 5009.3—2016. The study altered experimental conditions to explore key factors affecting constant weight in the direct drying method, optimized conditions for vacuum drying by adjusting vacuum pressure, and compared the effects of different reagents (xylene, Karl Fischer reagent) on detection results. Results In the direct drying method, sample temperature, cooling time in the desiccator and the degree of sample pulverization were identified as key factors affecting constant weight. For vacuum drying method, increasing the vacuum to -0.1 MPa and adding an effective desiccant to the drying box could rapidly evaporate moisture from the sample, improving detection efficiency. In the distillation method, the preparation and purification of analytical-grade toluene or xylene could be omitted. The Karl Fischer method could use a low-toxicity, pyridine-free Karl Fischer reagent. Conclusion The 4 detection methods in this standard are optimized separately to solve problems such as difficulty in achieving constant weight after repeated drying and the use of toxic and harmful reagents. The rationalization suggestions provide in this study have increased the operability of the standard and improved the testing efficiency of the laboratory.

moisture determination  /  national standard  /  key issues
孔芳, 李永刚, 刘小红, 张晓甜, 李国强, 袁超君, 侯力, 闻胜. GB 5009.3—2016《食品安全国家标准 食品中水分的测定》的关键问题探讨及方法优化. 食品安全质量检测学报, 2025 , 16 (13) : 189 -194 . DOI: 10.19812/j.cnki.jfsq11-5956/ts.20250103002
Fang KONG, Yong-Gang LI, Xiao-Hong LIU, Xiao-Tian ZHANG, Guo-Qiang LI, Chao-Jun YUAN, Li HOU, Sheng WEN. Exploration of key issues and method optimization of GB 5009.3—2016 National food safety standard-Determination of moisture in foods[J]. Journal of Food Safety & Quality, 2025 , 16 (13) : 189 -194 . DOI: 10.19812/j.cnki.jfsq11-5956/ts.20250103002
水分含量是食品加工和保存过程中的关键参数。食品中水分含量过高容易导致微生物滋生而缩短保质期[1-2]; 水分含量过低则可能影响食品的质地和口感[3-5], 同时食品水分含量的改变还会引起营养素及有害物质浓度的变化, 即同一食品可因水分的改变造成其他项目测定数据上的较大差异。因此, 水分含量的测定对于监控生产过程中的水分变化、优化产品配方和提高产品质量至关重要[6-8]
目前, 食品中水分含量检测主要有直接检测法和间接检测法[9]。直接检测法是基于食品在受热条件下水分自身游离易丢失的原理, 如烘箱干燥法、红外线干燥法、卤素灯干燥法等[10-12]; 间接检测法是利用水的化学反应或者水中的光折射、吸收、氢原子自旋、电磁波衰减等物理信号的变化来测定, 如卡尔·费休法[13-14]、蒸馏法、阿贝折射法、近红外光谱法[15-18]、低场核磁共振法[19-20]等。
我国现行有效的食品中水分测定相关的方法标准主要有GB 5009.3—2016《食品安全国家标准 食品中水分的测定》、GB/T 20264—2006《粮食、油料水分两次烘干测定法》、GB/T 26626—2011《动植物油脂 水分含量测定 卡尔·费休法(无吡啶)》等。其中GB 5009.3—2016是强制性标准, 包括直接干燥法、减压干燥法、蒸馏法和卡尔·费休法等4个方法。这4个方法在实际应用中仍存在一些问题, 例如干燥法中反复烘干难以达到恒重[21]、蒸馏法中甲苯、二甲苯及卡尔·费休法中含吡啶的卡尔·费休试剂有毒有害等[22-26]。本研究结合实验和数据对4个方法中的相关细节问题进行讨论和分析, 并提出了合理化建议, 为提高该标准在实际检测工作中的可操作性提供参考。
食品样品采购于武汉市的超市和农贸市场。玉米粉质控样(编号CFAPA-QC987B-1, 标准值11.975 g/100 g, 大连中食国实检测技术有限公司)。
甲苯、二甲苯、卡尔·费休试剂(含吡啶)、卡尔·费休试剂(无吡啶)、无水氯化钙(分析纯, 国药集团化学试剂有限公司)。
DHG-9143BS-Ⅲ型电热恒温干燥箱(上海新苗医疗器械制造有限公司); DZF-6020A型真空干燥箱(上海力辰科技有限公司); ZDJ-600S型全自动高精度滴定仪(北京先驱威锋有限公司); AL204型电子天平(精度0.01 mg, 瑞典梅特勒-托利多公司); Milli-Q去离子水发生器(美国Millipore公司)。
样品中水分含量测定参照GB 5009.3—2016进行。
所有数据均表示为同一批样品平行检测6次的平均值。实验室数据采用Microsoft Excel 2010对数据进行归类、分析和计算; 采用IBM SPSS Statistics 25.0进行成对样品t检验统计分析; 采用Microsoft Excel 2010软件绘图。
干燥法规定样品在烘箱内干燥的时间为2~4 h, 取出冷却后称量, 然后再干燥至恒重(前后两次质量差不超过2 mg)。该方法在实际使用过程中, 有实验室人员反映“存在难以达到恒重、需反复烘干、导致实验时间过长”等问题。本研究从样品温度、冷却时间长短、样品粉碎程度等方面来探索影响恒重的关键因素, 达到提高检测效率的目的。
对于高精度电子天平, 温度是影响天平准确度的重要因素[27-28]。样品在烘箱内干燥后仍处于高温状态, 若直接称量会由于高温导致电子天平不稳定, 从而出现数值漂移, 难以达到恒重。因此, 加热干燥后的样品应在干燥器内冷却至室温后再称量。
围绕加热干燥后的样品在干燥器内冷却时间的长短研究, 解决样品难以达到恒重的问题。
准确称取3 g玉米粉质控样品经过干燥4 h后, 在干燥器内冷却10 min、15 min、20 min、30 min、40 min、1 h后称量。结果显示, 当冷却时间小于15 min时, 称量瓶还处于微热状态, 称量时天平显示数值还不稳定; 当冷却时间为20 min时, 称量瓶已经冷却至室温状态, 称量时天平数值显示稳定。因此, 冷却时间至少需要20 min。
同时考察了当干燥器内湿度小于10%时, 准确称取3 g玉米粉质控样品经过干燥4 h冷却30 min后称量, 再继续干燥1 h后将样品放在干燥器内冷却30 min、1 h、2 h、4 h、8 h、16 h、96 h、192 h、288 h后称量, 连续两次干燥后称量的质量差的变化。结果如图1所示, 当冷却时间低于2 h时, 连续两次干燥后称定的质量差在2 mg内; 当冷却时间高于2 h时, 连续两次干燥后称定的质量差大于2 mg。这主要是因为干燥器内也并非是一个绝对干燥的环境, 变色硅胶经过了烘干处理, 使干燥器内的湿度小于10%, 当经过干燥处理的样品放入干燥器内, 会对干燥器中的水分进行一个再吸附再平衡, 放置时间(也就是冷却时间)越长, 可能导致样品中的水分在增加[29]
因此, 为了确保恒重, 同时满足节约时间、提高检测效率的目的, 建议干燥后样品的冷却时间严格控制在30 min。
GB 5009.3—2016中直接干燥法要求样品的干燥时间为2~4 h, 影响干燥时间的差别主要因素是样品粉碎后的粒径不同导致水分挥发速度不同[30]。本研究考察了玉米粉、茶叶和猪肉脯干在不同的干燥时间里对水分含量和恒重的影响情况。玉米粉、茶叶和猪肉脯干的粒径分别约为0.1、0.5、2.0 mm。准确称取3 g样品在103 ℃下分别干燥0.5、1.0、2.0、3.0、4.0、5.0、6.0 h后, 放入干燥器内冷却30 min后称量。结果如图2所示, 玉米粉、茶叶、猪肉脯干干燥时间分别为2.0、3.0、4.0 h时, 样品再次干燥后的质量差小于2 mg, 即已达到恒重。对于粒径大一些的猪肉脯干和茶叶, 样品内部水分难以挥发导致水分挥发的速度相对要慢一些, 达到恒重需要的时间要长。
同时考察了不同粒径的猪肉脯干在不同的干燥时间里对水分含量和恒重的影响情况。准确称取粒径分别为2、4、6、8 mm的猪肉脯干颗粒, 在103 ℃下分别干燥1、2、3、4、5、6、7、8、9、10 h后, 放入干燥器内冷却30 min后称量。结果如图3所示, 粒径越大, 猪肉脯干中水分的挥发速度越慢, 即达到恒重需要的时间越长。因此, 样品粒径也是影响干燥时间和恒重的重要因素。在样品制备过程中应尽可能将样品粉碎或研磨至细小颗粒状, 对于无法粉碎到更小粒径的食品基质应适当的延长首次干燥时间, 以减少复烘的次数。
GB 5009.3—2016规定, 减压干燥法的原理是在真空干燥箱达到一定压力(40~53 kPa)后加热至60 ℃±5 ℃下将样品中的水分去除。直接干燥法是在101.3 kPa, 温度101~105 ℃条件下加热样品将水分去除。理论上适用于直接干燥法的样品(如奶粉、玉米粉、淀粉等, 这3种基质均为粒径小于2 mm的均匀粉末状颗粒物, 基质中不含挥发性成分, 且含糖量低), 用减压干燥法测出的水分含量应与直接干燥法测出的结果一致, 但在实际操作过程中, 发现减压干燥法测定的结果均低于直接干燥法测定结果的20%左右。说明在压力为40~53 kPa下加热至60 ℃±5 ℃, 样品中的水分并没有完全被去除。同时, 在温度为60 ℃±5 ℃下, 真空干燥箱内的空气并不是绝对的干燥环境, 当样品中的水分含量与真空干燥箱内的水分含量一致时, 将达到一个水分平衡状态, 样品中的水分将无法继续被去除。这是导致测定结果偏低的主要原因。
为了优化减压干燥法的实验条件, 选取奶粉、玉米粉、马铃薯淀粉3种样品采用减压干燥法进行不同压力下和在有干燥剂的情况下测定水分的含量的试验比较, 同时用直接干燥法测定3种样品的水分含量。结果如表1所示, 当采用减压干燥法测定3种基质的水分时, 按照GB 5009.3—2016标准中减压干燥法规定的压力设置为50 kPa时, 测得的水分含量仅为直接干燥法的80%左右; 当压力设置为-0.1 MPa时, 测得的水分含量仅为直接干燥法的90%左右; 当压力设置为-0.1 MPa, 同时在真空干燥箱中加入无水氯化钙干燥剂时, 测得的水分含量为直接干燥法的95%左右。结果说明, 减压干燥法在压力为40~53 kPa下不足以把样品中的水分全部去除; 当把真空干燥箱中的压力调到最大值-0.1 MPa时, 样品中的水分也仅90%被去除; 当压力设置为-0.1 MPa, 同时在真空干燥箱内放入烘烤过的干燥剂时, 样品中的水分有近95%被去除。因此, 建议减压干燥法的压力应设置为-0.1 MPa, 并在真空干燥箱内加入有效干燥剂。
蒸馏法中使用的试剂为分析纯的甲苯或二甲苯, 方法中要求先对甲苯或二甲苯用水饱和后, 分去水层, 再进行蒸馏, 收集馏出液后备用。这两种试剂毒性较大, 短期吸入对眼及上呼吸道有刺激作用, 高浓度时对中枢神经系统有麻醉作用。根据GB/T 684—2023《化学试剂 甲苯》和GB/T 16494—2013《化学试剂 二甲苯》中的技术要求, 分析纯的甲苯和二甲苯的纯度要求分别为≥99.5%和≥99.0%, 水分含量均要求≤0.03%。本研究对分析纯甲苯和二甲苯进行了试剂空白检测(n=6), 因试剂中的含水量极低, 没有在水分接收管中接收到水分。同时考察了用蒸馏提纯过的二甲苯和未提纯过的二甲苯测定7种水果制品中的水分含量, 结果如表2所示, 未提纯和提纯过的分析纯二甲苯试剂测定7份样品中的水分结果的相对偏差为-1.36%~0.55%, 采用SPSS软件对2组数据进行t检验分析, P>0.05, 表明未提纯和提纯过的分析纯二甲苯试剂测定样品中的水分结果无显著性差异。因此, 建议分析纯的甲苯或二甲苯可不必采用蒸馏提纯的步骤, 既简化了实验步骤, 又可尽量减少检测人员接触甲苯或二甲苯试剂的时间。
卡尔·费休法中使用的是含吡啶的卡尔·费休试剂, 该试剂主要是由碘、二氧化硫、吡啶和甲醇组成的溶液, 吡啶在其中起催化作用。但是吡啶挥发性极强, 具有强烈的刺激性气味和毒性。现有研究发现采用无臭、无毒的咪唑类含氮氨碱或二乙醇胺可以替代吡啶官能团的作用[13-14]。本研究考察了含吡啶和无吡啶的卡尔·费休试剂对油脂和无水奶油中水分含量测定结果的影响, 重复测定6次, 评价采用无吡啶卡尔·费休试剂检测水分含量的精密度, 同时评价含吡啶和无吡啶的卡尔·费休试剂的测定结果的差异性。结果如表3所示, 采用无吡啶的卡尔·费休试剂测定样品中的水分含量的RSD为1.23%~1.38%, 精密度良好。通过SPSS软件, 对无吡啶的卡尔·费休试剂和含吡啶的卡尔·费休试剂的测定结果进行t检验分析, 结果显示两种试剂对检测结果无显著性差异, 即P>0.05。因此, 建议卡尔·费休法采用无吡啶的卡尔·费休试剂来替代含吡啶的卡尔·费休试剂, 以减少检测过程中有毒试剂对检测人员的身体伤害。
通过对GB 5009.3—2016标准中4个方法的操作步骤中的关键点及实验条件进行研究, 形成以下建议: (1)对于直接干燥法, 一是将样品粉碎或研磨至细小颗粒状或适当延长首次干燥时间, 以减少复烘的次数; 二是严格控制烘干后的样品放在干燥器内的冷却时间(30 min), 以快速达到恒重; (2)为了快速将食品中的水分挥发出来, 建议减压干燥法将真空度提高到-0.1 MPa, 并在干燥箱内加入有效干燥剂; (3)蒸馏法中的分析纯甲苯或二甲苯可删除试剂的制备提纯过程, 卡尔·费休法中采用毒性低的无吡啶卡尔·费休试剂, 以减少有毒有害试剂对实验人员身体和环境的危害。这些合理化建议增加了该标准的可操作性, 提高了实验室的检测效率, 为该标准的进一步修订提供了技术支持。
  • 国家重点研发计划项目(2023YFF1104800)
  • 2023年湖北省自然科学基金项目(2023AFB1019)
  • 国家卫生健康委食品安全国家标准修订项目(spaq-2022-28)
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2025年第16卷第13期
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doi: 10.19812/j.cnki.jfsq11-5956/ts.20250103002
  • 接收时间:2025-01-03
  • 首发时间:2026-01-12
  • 出版时间:2025-07-15
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  • 收稿日期:2025-01-03
基金
国家重点研发计划项目(2023YFF1104800)
2023年湖北省自然科学基金项目(2023AFB1019)
国家卫生健康委食品安全国家标准修订项目(spaq-2022-28)
作者信息
    1 湖北省疾病预防控制中心, 国家卫生健康委员会食品安全风险评估与标准研制特色实验室, 武汉 430079
    2 应城市疾病预防控制中心, 应城 432400

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*闻胜(1977—), 男, 博士, 研究员, 主要研究方向为食品安全。E-mail:
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2种不同金属材料的力学参数

Family
属数
Number of
genus
种数
Number of
species
占总种数比例
Percentage of
total species (%)

Genus
种数
Number of
species
占总种数比例
Percentage of total
species (%)
鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
小菇科 Mycenaceae 2 12 5.74 丝盖伞属 Inocybe 5 2.39
多孔菌科 Polyporaceae 8 14 6.70 蜡蘑属 Laccaria 5 2.39
红菇科 Russulaceae 3 23 11.00 小皮伞属 Marasmius 6 2.87
小菇属 Mycena 11 5.26
光柄菇属 Pluteus 5 2.39
红菇属 Russula 17 8.13
栓菌属 Trametes 5 2.39
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