[ Objective] The content of total antimony （Sb） in fresh fruit was investigated and its pollution was evaluated, to provide the basic data for diet exposure evaluation. [ Method] The content of total Sb in 194 sampl...[ Objective] The content of total antimony （Sb） in fresh fruit was investigated and its pollution was evaluated, to provide the basic data for diet exposure evaluation. [ Method] The content of total Sb in 194 samples was detected by hydride generation-atomic fluorescence spectrometry （HG-AFS）, and the Sb pollution in several fruits was evaluated by the method of single factor pollution index. [ Result ] The mean of total Sb was 0. 005 6 mg/kg, and the median was 0.003 8 mg/kg. The minimum value was not detected while the maximum value was O. 21 mg/kg, and the confidence interval was ND-O. 019 mg/kg （PS-P95）. The medi- ans of total Sb content in different fruits successively were dragon fruit （0.011 0 mg/kg） 〉 kiwi fruit （0.008 0 mg/kg） 〉 peach （0.006 0 mg/kg）. According to the method of single factor pollution index, the index from all samples was less than 0.2, suggesting that the samples involved were under the normal background value. [ Conclusion ] The Sb was detected in all samples but under the background value, and it was concluded that there was no Sb pollution in fresh fruit in Hunan Province.展开更多
[Objectives]To detect content of Pb,Cd,Hg,As,Cu,Zn,and Cr in Lysimachia christinae,and to analyze the pollution level.[Methods]Seven kinds of elements in L.christinae were determined by Inductively coupled plasma mass...[Objectives]To detect content of Pb,Cd,Hg,As,Cu,Zn,and Cr in Lysimachia christinae,and to analyze the pollution level.[Methods]Seven kinds of elements in L.christinae were determined by Inductively coupled plasma mass spectrometry and analyzed by single index and comprehensive index.[Results]The seven heavy metal elements showed good linearity in their respective concentration ranges.The recoveries of the samples were 84.5%-109.5%,and the RSD values were 2.30%-5.10%.Comparing the measured results of heavy metal elements with the limit values stipulated in the 2020 edition of the Chinese Pharmacopoeia and other standards,the Cr element in 19 batches of samples exceeded the standard,and the Zn element in 7 batches of samples exceeded the standard.The exceeding rates were 100.0%and 36.8%,respectively;the content of other heavy metal elements did not exceed the standard.The order of individual index from large to small was Cr,Zn,Cd,Hg,Cu,As,and Pb,and the average comprehensive pollution level was mild pollution and above.[Conclusions]L.christinae was mainly polluted by Cr,followed by Zn;this study can provide basic data for drafting of the limit standard for heavy metal elements in L.christinae.展开更多
目的采用一测多评(QAMS)法同时测定法制半夏曲中肌苷、鸟苷、腺苷等11种成分含量,并建立其灰色关联度分析(GRA)联合熵权逼近理想解排序分析法(EW-TOPSIS)综合质量评价方法。方法采用Shimadzu C 18色谱柱;乙腈-0.5%醋酸为流动相,梯度洗脱...目的采用一测多评(QAMS)法同时测定法制半夏曲中肌苷、鸟苷、腺苷等11种成分含量,并建立其灰色关联度分析(GRA)联合熵权逼近理想解排序分析法(EW-TOPSIS)综合质量评价方法。方法采用Shimadzu C 18色谱柱;乙腈-0.5%醋酸为流动相,梯度洗脱,流速1.0 mL·min-1;检测波长254和290 nm。以对甲氧基肉桂酸乙酯为内参比物质,计算其他10个成分的相对校正因子(RCF),测定各成分含量。采用GRA联合EW-TOPSIS模型对法制半夏曲进行综合质量评价。结果法制半夏曲中11种成分在一定浓度范围内线性关系良好,相关系数均>0.999;平均加样回收率96.94%~100.12%(RSD<2.0%,n=9);QAMS与外标法(ESM)实测值无明显差异。GRA模型相对关联度0.2903~0.6187,EW-TOPSIS模型相对接近度0.2114~0.6343;GRA和EW-TOPSIS模型综合评价结果基本一致。结论QAMS法便捷、准确,可用于法制半夏曲多指标成分定量控制,GRA联合EW-TOPSIS模型可用于法制半夏曲综合质量评价。展开更多
目的建立多指标结合化学计量学综合分析半夏天麻丸成分质量及关键指标的方法,为其质量评价提供科学依据。方法采用高效液相色谱一测多评(high performance liquid chromatography-quantitative analysis of multi-components by single-...目的建立多指标结合化学计量学综合分析半夏天麻丸成分质量及关键指标的方法,为其质量评价提供科学依据。方法采用高效液相色谱一测多评(high performance liquid chromatography-quantitative analysis of multi-components by single-marker,HPLC-QAMS)法建立12批半夏天麻丸11种成分含量测定方法,运用SPSS 26.0和SIMCA 14.0软件对以上指标进行聚类分析(clustering analysis,CA)、主成分分析(principal component analysis,PCA)及偏最小二乘-判别分析(partial least squares-discriminant analysis,PLS-DA),通过对12批产品的分析,综合评价半夏天麻丸质量及标志性成分。结果建立的11种成分含量测定方法稳定性较好。CA分析可将12批样品聚为三大类,2个主成分可代表11种成分92.142%的信息量,可用2个主成分对半夏天麻丸进行综合评价。根据PLS-DA结果分析,造成其质量差异的指标为橙皮苷、天麻素、柚皮芸香苷、毛蕊异黄酮葡萄糖苷和巴利森苷,可能是影响半夏天麻丸产品质量的差异性标志物。结论本实验首次建立了半夏天麻丸多指标成分质控方法,该方法易操作,重复性与稳定性良好;化学计量学手段也为半夏天麻丸质量控制研究提供了参考依据。展开更多
目的采用高效液相色谱一测多评(high performance liquid chromatography-quantitative analysis of multi-components by single marker,HPLC-QAMS)法同时检测延丹胶囊中10种主要成分含量,建立延丹胶囊多组分定量与化学计量学的综合分...目的采用高效液相色谱一测多评(high performance liquid chromatography-quantitative analysis of multi-components by single marker,HPLC-QAMS)法同时检测延丹胶囊中10种主要成分含量,建立延丹胶囊多组分定量与化学计量学的综合分析方法,构建延丹胶囊质量评控体系。方法采用Hedera ODS-2(C18)色谱柱,乙腈-0.1%冰醋酸为流动相,梯度洗脱,检测波长230 nm(检测3,29-二苯甲酰基栝楼仁二醇和3,29-二苯甲酰基栝楼仁三醇)和280 nm(检测二氢丹参酮Ⅰ、隐丹参酮、丹参酮Ⅰ、丹参酮ⅡA、原阿片碱、延胡索乙素、紫堇碱和四氢小檗碱);选取丹参酮ⅡA为内参比物质,建立其与其他9种成分的相对校正因子,计算各成分含量,同时运用外标法验证所建立HPLC-QAMS法的重复性、合理性和可行性;运用化学计量学方法对10批样品的10种成分含量数据进行分析,挖掘对其质量控制具有显著贡献的主要成分。结果定量分析的10种成分线性关系良好(r>0.999);平均加样回收率96.93%~100.14%(RSD<2.0%);HPLC-QAMS法所测结果与外标法无显著性差异;偏最小二乘-判别分析结果显示丹参酮ⅡA、3,29-二苯甲酰基栝楼仁三醇、丹参酮Ⅰ和延胡索乙素是影响延丹胶囊产品质量的差异性标志物(VIP值>1)。结论所建立的HPLC-QAMS多指标成分定量控制方法操作便捷,重复性与稳定性良好,结果准确可靠,结合化学计量学分析,可用于延丹胶囊的整体质量控制和综合评价。展开更多
基金Supported by Scientific Research Project of Medicine and Health Care in Hunan Province(B2014-162)Scientific Research Project of Xiangtan Science and Technology Bureau(SF20141003)
文摘[ Objective] The content of total antimony （Sb） in fresh fruit was investigated and its pollution was evaluated, to provide the basic data for diet exposure evaluation. [ Method] The content of total Sb in 194 samples was detected by hydride generation-atomic fluorescence spectrometry （HG-AFS）, and the Sb pollution in several fruits was evaluated by the method of single factor pollution index. [ Result ] The mean of total Sb was 0. 005 6 mg/kg, and the median was 0.003 8 mg/kg. The minimum value was not detected while the maximum value was O. 21 mg/kg, and the confidence interval was ND-O. 019 mg/kg （PS-P95）. The medi- ans of total Sb content in different fruits successively were dragon fruit （0.011 0 mg/kg） 〉 kiwi fruit （0.008 0 mg/kg） 〉 peach （0.006 0 mg/kg）. According to the method of single factor pollution index, the index from all samples was less than 0.2, suggesting that the samples involved were under the normal background value. [ Conclusion ] The Sb was detected in all samples but under the background value, and it was concluded that there was no Sb pollution in fresh fruit in Hunan Province.
基金Supported by Risk Monitoring Task Project of Chongqing Drug Administration in 2020。
文摘[Objectives]To detect content of Pb,Cd,Hg,As,Cu,Zn,and Cr in Lysimachia christinae,and to analyze the pollution level.[Methods]Seven kinds of elements in L.christinae were determined by Inductively coupled plasma mass spectrometry and analyzed by single index and comprehensive index.[Results]The seven heavy metal elements showed good linearity in their respective concentration ranges.The recoveries of the samples were 84.5%-109.5%,and the RSD values were 2.30%-5.10%.Comparing the measured results of heavy metal elements with the limit values stipulated in the 2020 edition of the Chinese Pharmacopoeia and other standards,the Cr element in 19 batches of samples exceeded the standard,and the Zn element in 7 batches of samples exceeded the standard.The exceeding rates were 100.0%and 36.8%,respectively;the content of other heavy metal elements did not exceed the standard.The order of individual index from large to small was Cr,Zn,Cd,Hg,Cu,As,and Pb,and the average comprehensive pollution level was mild pollution and above.[Conclusions]L.christinae was mainly polluted by Cr,followed by Zn;this study can provide basic data for drafting of the limit standard for heavy metal elements in L.christinae.
文摘目的采用一测多评(QAMS)法同时测定法制半夏曲中肌苷、鸟苷、腺苷等11种成分含量,并建立其灰色关联度分析(GRA)联合熵权逼近理想解排序分析法(EW-TOPSIS)综合质量评价方法。方法采用Shimadzu C 18色谱柱;乙腈-0.5%醋酸为流动相,梯度洗脱,流速1.0 mL·min-1;检测波长254和290 nm。以对甲氧基肉桂酸乙酯为内参比物质,计算其他10个成分的相对校正因子(RCF),测定各成分含量。采用GRA联合EW-TOPSIS模型对法制半夏曲进行综合质量评价。结果法制半夏曲中11种成分在一定浓度范围内线性关系良好,相关系数均>0.999;平均加样回收率96.94%~100.12%(RSD<2.0%,n=9);QAMS与外标法(ESM)实测值无明显差异。GRA模型相对关联度0.2903~0.6187,EW-TOPSIS模型相对接近度0.2114~0.6343;GRA和EW-TOPSIS模型综合评价结果基本一致。结论QAMS法便捷、准确,可用于法制半夏曲多指标成分定量控制,GRA联合EW-TOPSIS模型可用于法制半夏曲综合质量评价。
文摘目的采用高效液相色谱一测多评(high performance liquid chromatography-quantitative analysis of multi-components by single marker,HPLC-QAMS)法同时检测延丹胶囊中10种主要成分含量,建立延丹胶囊多组分定量与化学计量学的综合分析方法,构建延丹胶囊质量评控体系。方法采用Hedera ODS-2(C18)色谱柱,乙腈-0.1%冰醋酸为流动相,梯度洗脱,检测波长230 nm(检测3,29-二苯甲酰基栝楼仁二醇和3,29-二苯甲酰基栝楼仁三醇)和280 nm(检测二氢丹参酮Ⅰ、隐丹参酮、丹参酮Ⅰ、丹参酮ⅡA、原阿片碱、延胡索乙素、紫堇碱和四氢小檗碱);选取丹参酮ⅡA为内参比物质,建立其与其他9种成分的相对校正因子,计算各成分含量,同时运用外标法验证所建立HPLC-QAMS法的重复性、合理性和可行性;运用化学计量学方法对10批样品的10种成分含量数据进行分析,挖掘对其质量控制具有显著贡献的主要成分。结果定量分析的10种成分线性关系良好(r>0.999);平均加样回收率96.93%~100.14%(RSD<2.0%);HPLC-QAMS法所测结果与外标法无显著性差异;偏最小二乘-判别分析结果显示丹参酮ⅡA、3,29-二苯甲酰基栝楼仁三醇、丹参酮Ⅰ和延胡索乙素是影响延丹胶囊产品质量的差异性标志物(VIP值>1)。结论所建立的HPLC-QAMS多指标成分定量控制方法操作便捷,重复性与稳定性良好,结果准确可靠,结合化学计量学分析,可用于延丹胶囊的整体质量控制和综合评价。
