目的研制木薯乙醇和玉米乙醇中碳同位素标准物质,探讨碳同位素准确定值技术。方法定值分别采用元素分析-稳定同位素比质谱法(elemental analyzer-isotope ratio mass spectrometry,EA-IRMS)和液相色谱-稳定同位素比质谱法(liquid chroma...目的研制木薯乙醇和玉米乙醇中碳同位素标准物质,探讨碳同位素准确定值技术。方法定值分别采用元素分析-稳定同位素比质谱法(elemental analyzer-isotope ratio mass spectrometry,EA-IRMS)和液相色谱-稳定同位素比质谱法(liquid chromatography-isotope ratio mass spectrometry,LC-IRMS)。LC-IRMS分析过程中,将标准物质BCR657分别与待测样品和标准物质BCR660混合,可以实现对乙醇和蔗糖δ^13C值的同时测定。结果LC-IRMS方法验证结果显示使用该方法检测的标准物质BCR660的测量值在标准值的不确定度范围内,证明了混合检测方法的可行性。使用En值核查法对2种检测方法检测得到的乙醇样品δ13C值进行检验,|Encassava|=0.952,|Enmaize|=0.551,En值均小于1,证明2种检测方法所测结果等效一致。结论该方法不但有利于对乙醇进行多方法定值,且弥补了气相色谱-稳定同位素比质谱法(gas chromatography-isotope ratio mass spectrometry,GC-IRMS)标准物质有限的缺陷。本研究建立的分析技术和研制的标准物质可用于食品真实性鉴别。展开更多
Element analysis-mass spectrometry (EA-MS) is widely applied to determine samples' nitrogen isotopic composition in environmental and geological fields. In this research work, the suitable experimental conditions ...Element analysis-mass spectrometry (EA-MS) is widely applied to determine samples' nitrogen isotopic composition in environmental and geological fields. In this research work, the suitable experimental conditions for surface and loess sample measurement were chiefly ascertained. Further more, the negative influences in soil measurement,such as sample's uncompleted reaction, baseline excursion and the decline of oxidation capacity were stressed. The results show that the measurement precision of nitrogen isotopes can be hold less than ±0. 3‰, with Cr2O3/Co3O4Ag Oxidation Furnace, 80-90mL/min for Carrier-He flowrate, 80kPa for Conflo-He pressure and 100mL/min for Oxygen injection.展开更多
目的建立一种鉴别检测苹果汁掺假情况的元素分析/液相色谱-同位素比值质谱法(elemental analysis/liquid chromatography-isotope ratio mass spectrometry,EA/LC-IRMS)。方法通过对不同产区不同种类118个纯正苹果汁的糖、有机酸、果糖...目的建立一种鉴别检测苹果汁掺假情况的元素分析/液相色谱-同位素比值质谱法(elemental analysis/liquid chromatography-isotope ratio mass spectrometry,EA/LC-IRMS)。方法通过对不同产区不同种类118个纯正苹果汁的糖、有机酸、果糖、葡萄糖、二糖、寡糖碳同位素比值(δ^(13)C值)的测定,建立纯正苹果汁同位素数据库进而提出纯正苹果汁应满足的δ^(13)C值要求。结果有机酸和糖差值Δδ^(13)CO-S在-1.38‰至1.09‰范围内,果糖和葡萄糖差值Δδ^(13)CF-G在-0.70‰至0.57‰范围内,而各组分最大差值Δδ^(13)Cmax<4.36‰。对市售105个苹果汁进行检测,采用本方法检出32个阳性样品,而采用本实验室的糖浆标志物法仅检出12个阳性样品。结论本方法大大提高了苹果汁的掺假鉴别,有很大的实际应用潜力。展开更多
文摘目的研制木薯乙醇和玉米乙醇中碳同位素标准物质,探讨碳同位素准确定值技术。方法定值分别采用元素分析-稳定同位素比质谱法(elemental analyzer-isotope ratio mass spectrometry,EA-IRMS)和液相色谱-稳定同位素比质谱法(liquid chromatography-isotope ratio mass spectrometry,LC-IRMS)。LC-IRMS分析过程中,将标准物质BCR657分别与待测样品和标准物质BCR660混合,可以实现对乙醇和蔗糖δ^13C值的同时测定。结果LC-IRMS方法验证结果显示使用该方法检测的标准物质BCR660的测量值在标准值的不确定度范围内,证明了混合检测方法的可行性。使用En值核查法对2种检测方法检测得到的乙醇样品δ13C值进行检验,|Encassava|=0.952,|Enmaize|=0.551,En值均小于1,证明2种检测方法所测结果等效一致。结论该方法不但有利于对乙醇进行多方法定值,且弥补了气相色谱-稳定同位素比质谱法(gas chromatography-isotope ratio mass spectrometry,GC-IRMS)标准物质有限的缺陷。本研究建立的分析技术和研制的标准物质可用于食品真实性鉴别。
文摘Element analysis-mass spectrometry (EA-MS) is widely applied to determine samples' nitrogen isotopic composition in environmental and geological fields. In this research work, the suitable experimental conditions for surface and loess sample measurement were chiefly ascertained. Further more, the negative influences in soil measurement,such as sample's uncompleted reaction, baseline excursion and the decline of oxidation capacity were stressed. The results show that the measurement precision of nitrogen isotopes can be hold less than ±0. 3‰, with Cr2O3/Co3O4Ag Oxidation Furnace, 80-90mL/min for Carrier-He flowrate, 80kPa for Conflo-He pressure and 100mL/min for Oxygen injection.
文摘目的建立一种鉴别检测苹果汁掺假情况的元素分析/液相色谱-同位素比值质谱法(elemental analysis/liquid chromatography-isotope ratio mass spectrometry,EA/LC-IRMS)。方法通过对不同产区不同种类118个纯正苹果汁的糖、有机酸、果糖、葡萄糖、二糖、寡糖碳同位素比值(δ^(13)C值)的测定,建立纯正苹果汁同位素数据库进而提出纯正苹果汁应满足的δ^(13)C值要求。结果有机酸和糖差值Δδ^(13)CO-S在-1.38‰至1.09‰范围内,果糖和葡萄糖差值Δδ^(13)CF-G在-0.70‰至0.57‰范围内,而各组分最大差值Δδ^(13)Cmax<4.36‰。对市售105个苹果汁进行检测,采用本方法检出32个阳性样品,而采用本实验室的糖浆标志物法仅检出12个阳性样品。结论本方法大大提高了苹果汁的掺假鉴别,有很大的实际应用潜力。