CN106932393A - 一种日常防护型口罩中环氧乙烷残留量的测定方法及其评价方法 - Google Patents
一种日常防护型口罩中环氧乙烷残留量的测定方法及其评价方法 Download PDFInfo
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Abstract
本发明提供了一种日常防护型口罩中环氧乙烷残留量的测定方法及其评价方法。该环氧乙烷残留量的测定方法利用稀盐酸作为萃取剂,先后用高碘酸氧化萃取液并使用乙酰丙酮显色,最后用紫外分光光度计测定显色液的吸光度值。与现有技术相比,本发明具有前处理简单、测试结果稳定且检出限低、准确度高等优点,另外,本发明的方法填补了目前针对口罩产品中环氧乙烷残留量的检测空白,可用于检测各种材质的口罩中环氧乙烷的残留,具有一定的经济和社会效益。
Description
技术领域
本发明涉及化学有害物质的检测领域,具体涉及一种对日常防护型口罩中环氧乙烷残留量的比色分析测定方法及其评价方法。
背景技术
环氧乙烷(C2H4O)是一种广谱灭菌剂,可在常温下杀灭细菌、病毒、真菌等各种微生物,被广泛的应用在一次性输液器、口罩等器具的灭菌过程中。环氧乙烷本身对人体有很大的危害,接触后可能出现溶血、过敏反应等反应,长期接触高浓度的环氧乙烷可能导致组织坏死甚至致癌,加之口罩是直接与人体的呼吸系统接触的,因此口罩中的环氧乙烷残留将对人的健康带来严重的危害。在我国于近期实施的GB/T 32610-2016《日常防护型口罩技术规范》中明确规定了环氧乙烷残留量不得高于10ug/g。
《日常防护型口罩技术规范》要求经环氧乙烷处理的口罩按GB/T14233.1-2008中第9章的规定执行,采用气相色谱法-顶空进样技术进行分析,不过该方法对设备和技术要求均非常高,一般企业质检部门甚至是专业实验室可能无法满足测试条件。目前环氧乙烷残留量的测试常用的方法主要是碱性品红比色法,测试原理是环氧乙烷在酸性条件下水解成乙二醇,乙二醇经高锰酸钾氧化后生产甲醛,使用碱性品红与甲醛反应生成紫红色化合物,通过比色分析最终求得环氧乙烷的含量。不过该方法检出限较高,测试结果的重现性较差,尤其是在测定甲醛含量较低的样品时更明显,难以满足《日常防护型口罩技术规范》的技术要求。
发明内容
本发明提供了一种日常防护型口罩中环氧乙烷残留量的测定方法及其评价方法。该环氧乙烷残留量的测定方法利用稀盐酸作为萃取剂,先后用高碘酸氧化萃取液并使用乙酰丙酮显色,最后用紫外分光光度计测定显色液的吸光度值。
一种日常防护型口罩中环氧乙烷残留量的测定方法,具体步骤为:
(1)萃取试样:
a)将取自口罩的试样剪碎至5mm×5mm大小,称取样品0.5~2.0g加入到锥形瓶中,加入10~20mL浓度为0.05-0.2mol/L的盐酸,盖上瓶塞后放入超声装置中萃取30~60min,过滤得到萃取液;
b)从步骤a)所得萃取液中移取2mL溶液加入到比色试管中,再向每支试管中加入0.5~1.0mL浓度为5g/L的高碘酸溶液,充分混匀后静置30-60min,待其充分反应;
c)反应结束后分别向步骤b)的各试管中滴加浓度为100-200g/L的硫代硫酸钠溶液,此时溶液会缓慢变成黄色,继续滴加硫代硫酸钠至黄色消失,表明剩余的高碘酸已被反应完全;用0.05-0.2mol/L的盐酸将各试管内的混合溶液定容至5mL;加入5mL乙酰丙酮试剂,充分混合均匀后放入40℃水浴中显色30min,取出后在常温下避光冷却30min;
(2)配置标准溶液:以0.05-0.2mol/L的盐酸为溶剂,将已知浓度的乙二醇标准物质稀释配置成多个梯度浓度的标准工作溶液,按步骤(1)中b)和c)进行处理,并将乙二醇浓度折算为环氧乙烷的浓度;
(3)测试:用1~2cm的吸收池在分光光度计412nm波长处测定显色液的吸光度值,根据步骤(2)得到的多个梯度浓度的标准工作溶液显色后的吸光度值,建立环氧乙烷的浓度-吸光度值线性标准曲线,然后根据步骤(1)得到的显色样品溶液的吸光度查找出对应的环氧乙烷残留量。
进一步的,所述的乙酰丙酮试剂按以下操作配置:向1L容量瓶中加入150g的乙酸铵,用水溶解后加入3mL冰乙酸和2mL乙酰丙酮,用水稀释至刻度,用棕色瓶避光储存。
进一步的,所述环氧乙烷的浓度-吸光度值线性标准曲线的线性方程为Y=0.006x-0.002,相关系数R2=0.9995。
上述测定方法的评价方法为:
(1)精密度和回收率:量取乙二醇标准溶液加入到环氧乙烷阴性的样品中萃取和测试后,计算精密度和回收率,以重复7次测试标液吸光度值的相对标准偏差作为精密度,回收率计算公式为:
(2)检出限和定量限:斜率为k的线性曲线上最小浓度的标准溶液显色后重复测试6次,记录吸光度值及其标准偏差S,以3S/k值作为检出限,10S/k值作为定量限。
与现有技术相比,本发明的有益效果在于:
(1)本发明前处理操作简单,测试结果稳定,具有检出限低,回收率高等优点,能够满足GB/T 32610-2016《日常防护型口罩技术规范》中规定的技术要求。
(2)本发明的方法填补了目前针对口罩产品中环氧乙烷残留量的检测空白,可用于检测各种材质的口罩中环氧乙烷的残留,具有一定的经济和社会效益。
附图说明
图1为本发明提供的日常防护型口罩中环氧乙烷残留量的测定方法的实施例制定的环氧乙烷-吸光度标准曲线。
具体实施方式
下面结合实施例及其附图详细叙述本发明。实施例是以本发明所述技术方案为前提进行的具体实施,给出了详细的实施方式和方程,但本申请的权利要求保护范围不限于下属实施例的描述。
实施例1:
本方法对日常防护型口罩中环氧乙烷残留量进行了定量测试,具体步骤包括:
(1)萃取试样:
a)将试样按要求剪碎至5mm×5mm大小,准确称取代表性样品1.0g加入到锥形瓶中,加入10mL浓度为0.1mol/L的盐酸,盖上瓶塞后放入超声装置中萃取30min,过滤得到萃取液。
b)从步骤a)所得萃取液中准确移取2mL溶液加入到比色试管中,再向每支试管中加入0.5mL的高碘酸溶液(5g/L),充分混匀后静置30min,待其充分反应;
c)反应结束后分别向步骤b)的各试管中滴加硫代硫酸钠溶液(200g/L),此时溶液会缓慢变成黄色,继续滴加硫代硫酸钠至黄色消失,表明剩余的高碘酸已被反应完全。用0.1mol/L的盐酸将以上混合溶液定容至5mL;加入5mL乙酰丙酮试剂,充分混合均匀后放入40℃水浴中显色30min,取出后在常温下避光冷却30min;
(2)配置标准溶液:取一个干燥、清洁的50mL容量瓶,加水约30mL,精确称重。精确量取0.5mL乙二醇标准物质,迅速加入瓶中,摇匀,精确称重。计算前后两次质量差为0.564g,即为溶液中所含乙二醇的重量,加水至刻度,混匀得乙二醇储备液,并计算出乙二醇储备液的浓度为11.28g/L。将得到的储备溶液用0.1mol/L的盐酸稀释1000倍得浓度为11.28mg/L的乙二醇标准溶液,相当于环氧乙烷的浓度为8.01mg/L。从以上标准溶液中分别取0、0.125、0.25、0.5、1.0和2.0mL加入到比色管中,用0.1mol/L的盐酸定容至2.0mL,所得工作溶液中环氧乙烷浓度分别为0、0.50、1.00、2.00、4.00、8.01mg/L,将以上标准工作溶液按步骤(1)中b)和c)进行处理;
(3)测试:用1cm的吸收池在分光光度计412nm波长处测定显色液的吸光度值,建立环氧乙烷的浓度-吸光度值线性标准曲线,根据显色样品溶液的吸光度查找出对应的环氧乙烷残留量。各标准工作溶液显色后测得吸光度值见表1:
表1.各标准工作溶液显色后的吸光度值
经拟合可得线性方程为Y=0.006x-0.002,相关系数R2=0.9995,线性曲线见图1。
(4)精密度和回收率:准确量取适量乙二醇标准溶液,加入到环氧乙烷阴性的样品中萃取,测试,计算精密度和回收率,以测量7次标准溶液吸光度值的相对标准偏差作为精密度,并计算回收率,结果见表2:
表2.不同浓度下环氧乙烷的回收率和精密度
(5)检出限和定量限:向比色管中移取0.125mL乙二醇,用0.1mol/L的盐酸定容至2mL,按步骤(1)中b)和c)进行处理;显色后重复测试6次,吸光度值分别为0.020、0.022、0.024、0.024、0.025、0.026,计算其标准偏差S=0.002,进而得到该方法的检出限为3S/k=1.0ug/g,定量限为10S/k=3.4ug/g。
以上数据显示本方法的平均回收率主要在80~100%区间,相对标准偏差均小于10%,结果在可接受的范围内,定量限小于满足《日常防护型口罩技术规范》的技术要求,表明本方法可完全满足日常测试要求。
可以理解的是,以上是为了阐述本发明的原理和可实施性的示例,本发明并不局限于此。对于本领域内的普通技术人员而言,在不脱离本发明的精神和实质的情况下,可以做出各种变型和改进,这些变型和改进也视为本发明的保护范围。
Claims (4)
1.一种日常防护型口罩中环氧乙烷残留量的测定方法,其特征在于,具体步骤为:
(1)萃取试样:
a)将取自口罩的试样剪碎至5mm×5mm大小,称取样品0.5~2.0g加入到锥形瓶中,加入10~20mL浓度为0.05-0.2mol/L的盐酸,盖上瓶塞后放入超声装置中萃取30~60min,过滤得到萃取液;
b)从步骤a)所得萃取液中移取2mL溶液加入到比色试管中,再向每支试管中加入0.5~1.0mL浓度为5g/L的高碘酸溶液,充分混匀后静置30-60min,待其充分反应;
c)反应结束后分别向步骤b)的各试管中滴加浓度为100-200g/L的硫代硫酸钠溶液,此时溶液会缓慢变成黄色,继续滴加硫代硫酸钠至黄色消失,表明剩余的高碘酸已被反应完全;用0.05-0.2mol/L的盐酸将各试管内的混合溶液定容至5mL;加入5mL乙酰丙酮试剂,充分混合均匀后放入40℃水浴中显色30min,取出后在常温下避光冷却30min;
(2)配置标准溶液:以0.05-0.2mol/L的盐酸为溶剂,将已知浓度的乙二醇标准物质稀释配置成多个梯度浓度的标准工作溶液,按步骤(1)中b)和c)进行处理,并将乙二醇浓度折算为环氧乙烷的浓度;
(3)测试:用1~2cm的吸收池在分光光度计412nm波长处测定显色液的吸光度值,根据步骤(2)得到的多个梯度浓度的标准工作溶液显色后的吸光度值,建立环氧乙烷的浓度-吸光度值线性标准曲线,然后根据步骤(1)得到的显色样品溶液的吸光度查找出对应的环氧乙烷残留量。
2.根据权利要求1所述的日常防护型口罩中环氧乙烷残留量的测定方法,其特征在于,所述的乙酰丙酮试剂按以下操作配置:向1L容量瓶中加入150g的乙酸铵,用水溶解后加入3mL冰乙酸和2mL乙酰丙酮,用水稀释至刻度,用棕色瓶避光储存。
3.根据权利要求1或2所述的日常防护型口罩中环氧乙烷残留量的测定方法,其特征在于,所述环氧乙烷的浓度-吸光度值线性标准曲线的线性方程为Y=0.006x-0.002,相关系数R2=0.9995。
4.一种用于评价权利要求1所述的日常防护型口罩中环氧乙烷残留量的测定方法的方法,其特征在于,包括以下指标:
(1)精密度和回收率:量取乙二醇标准溶液加入到环氧乙烷阴性的样品中萃取和测试后,计算精密度和回收率,以重复7次测试标液吸光度值的相对标准偏差作为精密度,回收率计算公式为:
(2)检出限和定量限:斜率为k的线性曲线上最小浓度的标准溶液显色后重复测试6次,记录吸光度值及其标准偏差S,以3S/k值作为检出限,10S/k值作为定量限。
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