Study on residues of heavy metals and harmful elements in Qingqiao and Laoqiao based on chemometrics / 中国中药杂志

Forsythiae Fructus is divided into Qingqiao and Laoqiao due to different harvesting periods. So far, the accumulation of heavy metals in the two types of Forsythiae Fructus has not been reported. In this study, the residual levels of copper(Cu), lead(Pb), chromium(Cr), arsenic(As), cadmium(Cd) and mercury(Hg) in 29 batches of Laoqiao and 60 batches of Qingqiao were determined by inductively coupled plasma mass spectrometry(ICP-MS). The samples were collected from Shanxi, Shaanxi, Henan, and Hebei Provinces. In addition, the diversity and correlation of harmful elements in Qingqiao and Laoqiao were analyzed by multivariate statistical method. Furthermore, principal component analysis(PCA) was used to analyze the harmful elements concentrations of Qingqiao and Laoqiao. The results showed that there was a significant difference on the residual levels of heavy metals and harmful elements between Qingqiao and Laoqiao. Among them, the content of Pb in Laoqiao is significantly higher than that in Qingqiao(P<0.01), while the content of Cu is significantly lower than that in Qingqiao. However, the difference in harmful elements among different producing areas of Forsythiae Fructus is not significant. PCA analysis showed that Qingqiao and Laoqiao were successfully grouped into two categories. This study suggests significant difference in the residual levels of heavy metals and harmful elements between Qingqiao and Laoqiao. Besides, Forsythiae Fructus has a certain enrichment of Pb in the fruit ripening stage(Laoqiao). This study provides a reference for the quality classification and safety of Forsythiae Fructus.

Study on quality status of mineral medicine Calamina / 中国中药杂志

In this paper, some quality problems of mineral medicine Calamina and calcined Calamina have been discussed after determination and analysis of the quality parameters of a large number of market samples, and the countermeasures are put forward. According to the XRD results, as well as the results of tests included in Chinese Pharmacopoeia(2015 edition), the authenticity of Calamina and calcined Calamina samples were identified. The content of zinc oxide in samples were determined by the method of determination in Chinese Pharmacopoeia. Individually, inductively coupled plasma mass spectrometry(ICP-MS), inductively coupled plasma atomic emission spectrometry(ICP-AES) and atomic fluorescence spectrometry(AFS) methods were used for the determination of impurity elements and harmful elements in Calamina and calcined Calamina samples. Four kinds of impurity elements of magnesium(Mg), iron(Fe), aluminum(Al), calcium(Ca) and five harmful elements such as lead(Pb), cadmium(Cd), arsenic(As), copper(Cu), mercury(Hg) were measured. The study showed that: ① Fake Calamina products on the market were overflowing; ② The mineral origin of the mainstream Calamina in the market is inconsistent with that stipulated in Chinese Pharmacopoeia(2015 edition); ③ The contents of harmful elements Pb and Cd in Calamina and calcined Calamina are generally higher, while the contents of harmful elements As and Cu in some inferior Calaminae are higher; ④ Parts of calcined Calamina were improperly or inadequately processed. In view of these quality problems, the countermeasures are put forward as follows: ① It is suggested that hydrozincite should be approved as the mineral source of Calamina, and be included by Chinese Pharmacopoeia; ② Strengthen the research on the specificity of Calamina identification methods to improve the quality control level; ③ Strengthen the research on the processing of Calamina, and formulate the limit standards for the content of Pb and Cd in Calamina; ④ Carry out research on the artificial synthesis of Calamina and calcined Calamina, in order to cope with the current shortage of Calamina resources and ensure the sustainable development of Calamina medicinal materials.

Current situation of heavy metal pollution,detection and removal techniques in medicinal marine organisms in China / 中国中药杂志

As an important branch of traditional medicines,medicinal marine organisms have many advantages,including biological diversity,remarkable biological activity,especial for the treatment of anti-cancer,anti-virus,anti-coagulation,analgesia,anti-bacterial,cardiovascular and cerebrovascular diseases. In recent years,with the continuous exploration of marine organisms by human beings,many marine organisms with specific biological activities and medicinal prospects have been found,which have attracted great attention around the world and thus called " new hope" to solve human health problems. However,due to the rapid development of modern industry,heavy metal pollution not only poses a great threat to medicinal marine living resources,but also hinders the development of marine biomedical industry and threatens human health. In view of this,this paper introduced the development trend of medicinal marine organisms and the current situation of heavy metal pollution and focusing on the analysis technology and chemical removal technology of heavy metals in medicinal marine organisms,which is to provide reference for the heavy metals control in marine medicines and the development and utilization of marine medicines.

Determination and risk assessment of heavy metals and harmful elements residues in Niuhuang Qingwei Pills based on ICP-MS / 中国中药杂志

To achieve a comprehensive understanding of heavy metals and harmful elements residues in Niuhuang Qingwei Pills,49 samples from 18 manufactures were collected from 31 provinces in China.Risk assessment and control preparations were applied innovatively in evaluation of exogenous pollution in traditional Chinese Medicine.Determination methods for Pb,Cd,As,Hg and Cu were established by inductively coupled plasma mass spectrometry(ICP-MS).Based on the procedures including hazard identification,hazard characterization,exposure assessment and risk characterization,risk assessment was performed and residual limits for Pb,Cd,As,Hg and Cu in the drug were formulated.The results showed that the hazardous quotients(HQ) of the elements were decreased in the following order:Pb>As>Cu>Hg>Cd,and the total hazardous index(HI) of heavy metals and harmful elements in Niuhuang Qingwei Pills was above 1,implying health risk of the drug.Under the proposed limits,5 elements in the control preparation as well as Cd and Cu in the samples were within the limits range,but the excess rates of Pb,As and Hg in the samples were 12%,12% and 14%,respectively.For the first time,basic steps for risk assessment of Chinese patent medicine were established,which provided model and reference for risk assessment and limit formulation of other drugs.

Discussion on evaluation mode of proficiency testing for heavy metal and harmful element detection in medicines / 中国中药杂志

This study aims to explore the evaluation model for the proficiency testing of heavy metal and harmful element residues in pharmaceuticals,and to provide reference for the proficiency testing program and proficiency testing result in the field of residue analysis. The proficiency test result of cadmium determination in honeysuckle as an example. The algorithm A,NIQR,and Horwitz function are used to calculate the assigned value and the standard deviation. Z was obtained at the same time. If | Z | ≤2,the result is satisfactory. If 2< | Z | <3,the result is questionable. If | Z | ≥3,the result is unsatisfactory. In addition,the median value is the assigned value,and deviation(D%) is used. If D% is not more than 16%,the result is satisfactory; if D% is more than 16%,the result is unsatisfactory. After analysis,in the results of questionable or dissatisfied laboratories calculated by algorithm A and NIQR,the deviation error of some data is within the scope of the standard. In the results of the satisfactory laboratory evaluated by the Horwitz function,some data deviation errors far exceed the standard range. The evaluation result of the D% meets the requirements. According to heavy metal and harmful element trace analysis methods,this study is the first to apply D% to the evaluation of the detection ability of heavy metals and harmful elements in pharmaceuticals. This method makes the evaluation result more reasonable,and has important reference significance for the evaluation of other proficiency test results.

Determination of Antiseptic, Residual Ethanol, Heavy Metals and Harmful Elements in Fuyanyu Mixture / 中国药师

Objective:To study the safety factors of Fuyanyu mixture. Methods: The contents of antiseptic and residual ethanol were determined by HPLC and GC, respectively, and those of heavy metals and harmful elements were detected by ICP-MS. Results:The contents of benzoic acid in 6 batches of samples were less than 0. 3%. In two thirds of samples, ethanol residue was more than 0. 5%. The total mercury exceeded 15μg/day in one of the samples, and the contents of Pb, Ge, Gr, As, Ni and Cu met the limits described in USP<232> in all of the last samples. Conclusion: The methods are accurate and reliable. It is urgent to improve the preparation process so as to reduce the residual amount of ethanol according to the detection results. It is recommended to increase the testing items that affect the safety of the preparation so as to control the preparation quality strictly.

Determination of Antiseptic, Residual Ethanol, Heavy Metals and Harmful Elements in Fuyanyu Mixture / 中国药师

Objective:To study the safety factors of Fuyanyu mixture. Methods: The contents of antiseptic and residual ethanol were determined by HPLC and GC, respectively, and those of heavy metals and harmful elements were detected by ICP-MS. Results:The contents of benzoic acid in 6 batches of samples were less than 0. 3%. In two thirds of samples, ethanol residue was more than 0. 5%. The total mercury exceeded 15μg/day in one of the samples, and the contents of Pb, Ge, Gr, As, Ni and Cu met the limits described in USP<232> in all of the last samples. Conclusion: The methods are accurate and reliable. It is urgent to improve the preparation process so as to reduce the residual amount of ethanol according to the detection results. It is recommended to increase the testing items that affect the safety of the preparation so as to control the preparation quality strictly.

Determination of heavy metals and harmful elements in Yuanhu zhitong capsule / 中国生化药物杂志

Objective To determine the content of heavy metals and harmful elements in commercially available Yuanhu Zhitong Capsule. Methods The determination of lead, cadmium, arsenic, mercury, copper and chromium by atomic absorption spectrometry and atomic fluorescence spectrometry was established.Results The recovery rate of the method was between 91.2% and 111.2%, and the precision of the experiment was less than 5%, and the range of each element was good.The stability and reproducibility of the method were good.Lead and cadmium and copper of Yuanhu zhitong capsule in different degree exceeded the standard, while the content of arsenic, mercury and chromium was in accordance with the requirements. Conclusion The method is simple and easy to operate, convenient and quick.The content of the current limit of Yuanhu zhitong capsule still need to establish the quality standard of lead and cadmium, arsenic, mercury, copper and chromium.In this paper, the establishment of the heavy metals and harmful elements determination method of Yuanhu zhitong capsule provide quality control and safety evaluation of reference.

Research advances on detecting heavy metals and harmful elements based on fluorescent probe quantum dots / 中草药

In recent years, it is a hot spot of research on detecting heavy metals such as Pb (II), Cu (II), and Hg (II) and harmful element As (III) based on novel fluorescence probe quantum dots (QDs). This review introduced the preponderance optical properties and advantages of QDs. In addition, the principles of fluorescence quenching concerning ion complexing reaction, electron transfer, fluorescence resonance energy transfer and others, fluorescence enhancement and methods combined with rolling circle amplification of DNA, redshift of emission wavelength, fluorescence ratio and others were presented. Finally, the paper summarized the applications and took prospect to provide the basis for the detections of heavy metals and harmful elements in Chinese materia medica based on fluorescence probes QDs.

Determination of Five Heavy Metals and Harmful Elements in Freeze-dried Rehmannia from Different Habitats / 中国药师

Objective:To analyze the content of Pb, Cd, Cu, As and Hg in freeze-dried Rehmannia from different habitats by FAAS and double channels AFS. Methods:The contents of Pb,Cd and Cu in Rehmannia from different habitats were directly deter-mined by FAAS, while the contents of As and Hg were determined by double channels AFS after pretreated with HNO3-HClO4 . Re-sults:It was shown that each element had good linear relationship with the correlation coefficient above 0. 997 4. The average recovery was 97. 88%-100. 90% with RSD of 0. 019% -4. 20% (n=6). Meanwhile, the concentrations of 5 harmful elements and heavy met-als in 4 batches of 10 samples were higher than the limits described in Chinese pharmacopoeia. Conclusion:The results measured by the method are considered to be accurate, quick and easy to be operated. It can be used to determine heavy metals and harmful ele-ments in freeze-dried Rehmannia from different habitats.

Discussion of Quality Control of She Medicine -Melastoma Dodecandrum / 中国药师

Objective: To discuss the quality control method and index of traditional She medicine -Melastoma dodecandrum. Methods:The contents of gallic acid , ellagic acid and total flavonoids ( the total amount of quercetin and kaempferol) were deter-mined by HPLC. Water content, acid insoluble ash content, extract, heavy metals and harmful elements in 26 batches of herbs were also detected. Results:The content range of gallic acid, ellagic acid and total flavonoids was 9. 84-26. 31 mg·g-1 , 4. 13-16. 11 mg· g-1 and 1. 31-38. 28 mg · g-1 , respectively. The content range of water, acid insoluble ash and extract was 6. 70%-13. 90%, 1. 05%-6. 20% and 18. 00%-40. 80%, respectively. The content of Pb in all the samples was more than 5 ppm, the number of sam-ples with the content of Cd above ten thousand three was 7, and the content of As, Hg and Cu in all the samples was less than 1 ppm, ten thousand one and 20 ppm, respectively. Conclusion:The contents of gallic acid, ellagic acid and total flavonoids can comprehen-sively reflect the content of active ingredients in Melastoma dodecandrum. The contents of acid insoluble ash, Pb and Cd in Melastoma dodecandrum are relative high, which should be studied further to draw up reasonable limit.