Analysis of the of Pb, Cd and As in decoction of Lindera aggregata (Sims) Kosterm. by PBET digestion in vitro/Caco-2 cell model and their cumulative risk assessment / 药学学报

Inductively coupled plasma mass spectrometry (ICP-MS) was applied to determine the concentrations of lead (Pb), cadmium (Cd) and arsenic (As) in Lindera aggregata (Sims) Kosterm. The physiologically based extraction test (PBET) digestion in vitro/Caco-2 cell model was established to investigate the bioaccessible contents of Pb, Cd and As in decoction of Lindera aggregata (Sims) Kosterm. The target-organ toxicity dose modification of HI method (TTD) was used to evaluate the cumulative risk caused by the combined exposure of the total levels of Pb, Cd and As in Lindera aggregata (Sims) Kosterm. and the bioaccessible contents in the decoction. The results showed that the total contents of Pb, Cd and As in 4 batches of samples were in the range of 2.901-3.872, 1.299-1.800 and 0.062-0.216 mg·kg-1, respectively. After transportation by Cacco-2 cells, the bioaccessible contents of Pb, Cd, and As in the decoction were in the range of 0.045-0.080, 0.070-0.112 and 0.004-0.018 mg·kg-1. The results of risk assessment showed that calculated by the total amounts of heavy metals in the Lindera aggregata (Sims) Kosterm., for the end points of nervous system, the cumulative risks of co-exposure of heavy metals in 3 batches of samples were of concern. After decoction and transportation by Caco-2 cells, for the end points of cardiovascular system, blood, nervous system, kidney and testis, the TTD modification of HI values of all batches of samples were less than 1, and the health risks were acceptable. The study provided methodology basis for a more objective assessment of the health risks of heavy metals and harmful elements in traditional Chinese medicine and for a more scientific limit standard of heavy metals and harmful elements.

Current situation and problems of national standards for Chinese medicinal materials / 中国中药杂志

To learn the current situation and strengthen the management of national standards for Chinese medicinal materials, we sorted out the relevant national standards. According to incomplete statistics, there are 1 185 kinds of Chinese medicinal materials, including 1 024 kinds of plant medicines, 106 kinds of animal medicines, and 54 kinds of mineral medicines, in addition to ethnic medicinal materials with different functions. The relevant standards include 819 Pharmacopoeia standards, 342 standards issued by the Ministry of Health or National Medicinal Products Administration, 7 standards for new medicinal materials, and 17 standards for imported medicinal materials. In this paper, the sources of standards as well as the distribution of families and genera and the distribution of medicinal parts of medicinal materials are analyzed. The suggestions are as follows:(1)to improve the coordination among different national standards of Chinese medicinal materials;(2)to improve the standardization and controllability of relevant standards;(3)to revise the issued standards for Chinese medicinal materials(including Tibetan, Uygur, and Mongolian medicinal materials).

[Comparison between charged aerosol detector and evaporative light scattering detector for analysis of sugar in Zhusheyong Yiqi Fumai and study on accuracy of methods].

Evaporative light scattering detector(ELSD) and charged aerosol detector(CAD) methods were established in this study for the content determination of four kinds of sugars in Zhusheyong Yiqi Fumai(YQFM), and the factors affecting the accuracy of CAD methods were discussed. HPLC-ELSD chromatographic separation was performed on a Shodex Asahipak NH2 P-50 column with acetonitrile-water(75∶25)as the mobile phase, with a flow rate of 0.8 mL·min~(-1), drift tube temperature of 80 ℃. The analysis by HPLC-CAD was performed on the same column with acetonitrile-water as mobile phase for gradient elution, with a flow rate of 0.8 mL·min~(-1), a neb temperature of 45 ℃, and power function(PF) of 1.3. The samples of YQFM were detected by ELSD and CAD respectively. It was found that YQFM was composed of fructose, glucose, sucrose and maltose. The linear relationship of the two methods was good, and the recoveries, reproducibility and stability of these four kinds of sugars measured by the two methods satisfied the requirements of methodology. Both CAD and ELSD detectors were accurate and reliable in detecting saccharides components in YQFM. In addition, it was revealed in this study for the first time that the PF parameter of CAD had an important influence on the accuracy of sugar determination and acted as the key parameter of CAD method. It was also found that for CAD, a non-linear detector, there was no significant difference between the results of linear regression and logarithmic regression.

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.

Screening of multiple pesticide residues in Jinyinhua Formula Granules / 中国中药杂志

To evaluate the pesticide residue risk of Jinyinhua Formula Granules( made from Lonicerae Japonicae Flos) used in the market preliminarily,20 samples of Jinyinhua Formula Granules from 5 manufactures were collected randomly through the national evaluative sampling test program. Totally 262 pesticides( involving 270 chemical monomers) with monitoring significance to traditional Chinese medicinal materials were detected. Samples were extracted by high speed homogenate with acetonitrile as solvent. And their residues were analyzed by GC-MS/MS and LC-MS/MS in MRM mode. No less than 2 groups of characteristic ion pairs were adopted for qualitative detection,and the calibration curve method was used for quantitative detection. The results showed that 20 pesticides were detected in 20 batches of Jinyinhua Formula Granules,with an average of about 9 pesticides detected in every batch,but no restricted pesticide was detected. The detected pesticides were all at the trace level,which was far lower than the limit of the general food standard. Therefore,the safety risk was low in Jinyinhua Formula Granules. In this study,a screening method for pesticide residues in Jinyinhua Formula Granules was established for the first time. The method was accurate and rapid,and the detection indicators were highly targeted. The results could provide theoretical reference for the prevention and control of pesticide safety risks in Jinyinhua Formula Granules and even traditional Chinese medicine formula granules.

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.

Risk assessment of pesticide residues in domestic ginsengs / 中国中药杂志

The study aims at taking risk assessment of pesticide residues in ginseng and high risk pesticides were picked up in order to provide a scientific basis for the establishment of maximum residue limits(MRLs) for pesticides in ginseng. Residues of 246 pesticides in 80 ginseng samples collected from different place were detected by GC-MS/MS and LC-MS/MS method. Acute and chronic intake risks were evaluated by using deterministic approach, and the matrix ranking developed by the Veterinary Residues Committee of the United Kingdom was referred to assess risk score of pesticides. The 25 kinds of pesticide residues were detected in ginseng samples, the detection rate of quintozene(PCNB) was 78%, which was the most frequently detectable pesticide. The chronic dietary intake risks of 25 pesticide residues expressed as %ADI were 0.00%-2.6%, and their acute dietary intake risks expressed as %ARfD were 0.00%-104.2%. Among them the acute dietary intake risks of PCNB was 104%,which was the highest. The 25 pesticides were divided into 3 groups by risk score, high risk group(4 pesticides), medium risk group(6 pesticides), and low risk group(15 pesticides). Hexachlorobenzene, phorate, PCNB and BHC were classified as high risk group. It is necessary and effective to establish the limit of residual organic chlorine in ginseng from Chinese Pharmacopoeia(2015 edition). MRLs for PCNB and hexachlorobenzene in ginseng were proposed to be revised based on the results of risk assessment.

Risk Assessment of Arsenic Exposure by Chinese Materia Medica in Chinese Population / 中国中医药信息杂志

Objective To analyze the intake of arsenic in Chinese materia medica by Chinese population; To assess its health risk. Methods Totally 2056 Chinese materia medica samples were collected from representative manufacturers and markets in China from 2008 to 2016 and their arsenic contents were detected. The consumption data of Chinese materia medica were collected among population aged 18 and above from 5739 individuals by face to face questionnaire surveys in 5 provinces (Heilongjiang, Liaoning, Jiangxi, Guizhou and Gansu) with the method of multistage stratified random sampling. A deterministic estimate was used to assess the exposure of arsenic by Chinese materia medica. At the same time, the Chinese standard limit of arsenic in Chinese materia medica was used to do the theory assessment. Results The average concentration of arsenic in Chinese materia medica was 0.81 mg/kg. The residue level of arsenic in animal Chinese materia medica (average concentration: 3.29 mg/kg) was higher than that in medicinal plants (average concentration: 0.71 mg/kg). The consumption data showed that average intake of Chinese materia medica as medicines was 207 g, and P95was 540 g; the average intake of Chinese herbals as medicinal food was 43 g, and P95was 500 g. The assessment using arsenic content data showed that common use of Chinese materia medica had low level of risk. However, the population with chronic and high consumption of Chinese materia medica as medicine or as food had certain level of health risk. Arsenic content in animal herbals was about 5 times higher than that of medicinal plants. But according to the consumption, the risk was not higher than that of medicinal plants. The assessment using the standard limit of arsenic (2 mg/kg) in herbals showed that recent standard could protect most people, but risk remained in those with chronic consumption of Chinese materia medica as medicineand high consumption of Chinese materia medica as medicinal food. Conclusion The current standard limit of arsenic (2 mg/kg) in Chinese materia medica is appropriate. The health risk of arsenic exposure from Chinese materia medica among Chinese population is at a low level, but those with chronic and high Chinese materia medica consumption need more attention.

Determination of polycyclic aromatic hydrocarbons in traditional Chinese medicines by isotope dilution gas chromatography-tandem mass spectrometry / 中国药学杂志

OBJECTIVE: To develop a GC-MS/MS method for the determination of the residues of 16 polycyclic aromatic hydrocarbons (PAHs) in Chinese herbal medicines. METHODS: Using isotope as internal standard, the sample was extracted by ethyl acetate and purified by solid phase extraction on C18 cartridges. GC-MS/MS method was used for the assay, with analyte protectants added to counteract the matrix effect. The chromatographic column was DB-5ms(0.25 mm × 30 m, 0.25 μm) with temperature programming and MRM detection. RESULTS: The calibration curves for the 16 kinds of typical PAHs were linear in the range of 1 - 100 ng · mL-1. The average recovery rate was 88.53% - 119.03% in the range of 1 -25 μg · kg-1 with RSDs of 1.25% - 14.70% (n = 3). The LOQs were 0.2 - 1 μg · kg-1. CONCLUSION: This method is specific, sensitive, accurate and can be used for residue detection of 16 typical kinds of PAHs in Chinese herbal medicines.

Census of pesticide residues and suggestions for control in traditional Chinese medicine / 中国中药杂志

In our study, 198 types of pesticides in 120 types 333 lots of traditional Chinese medicine (TCM), which were reasonably classified according to its matrix property, were determined by using the pretreatment platform and gas chromatography-mass spectrometry method. As a result, 158 were contaminated with pesticides. However, the content of pesticides in most TCM was very low. In addition, types of pesticides were different in different part of materia medica. In conclusion, the current status of pesticide residues pollutants in TCM was summarized, and the result can provide proof for the formulation of maximum residue limit. The new species of herbs and the new detecting index should be electively monitored in Chinese Pharmacopeia.

Quality assessment of sulfur-fumigated paeoniae alba radix / 中国中药杂志

The samples of sulfur-fumigated Paeoniae Alba Radix acquired both by random spot check from domestic market and self-production by the research group in the laboratory were used to evaluate the effects of sulphur fumigation on the quality of Paeoniae Alba Radix by comparing sulfur-fumigated degree and character, the content of paeoniflorin and paeoniflorin sulfurous acid ester, and changes of the fingerprint. We used methods in Chinese Pharmacopeia to evaluate the character of sulfur-fumigated Paeoniae Alba Radix and determinate the content of aulfur-fumigated paeoniflorin. LC-MS method was used to analyze paeoniflorin-converted products. HPLC fingerprint methods were established to evaluate the differences on quality by similarity. Results showed that fumigated Paeoniae Alba Radix became white and its unique fragrance disappeared, along with the production of pungent sour gas. It also had a significant effect on paeoniflorin content. As sulfur smoked degree aggravated, paeoniflorin content decreased subsequently, some of which turned into paeoniflorin sulfurous acid ester, and this change was not reversible. Fingerprint also showed obvious changes. Obviously, sulfur fumigation had severe influence on the quality of Paeoniae Alba Radix, but we can control the quality of the Paeoniae Alba Radix by testing the paeoniflorin sulfurous acid ester content.

Inhibitory effect of cinnamon powder on pathogen growth in laboratory media and oriental-style rice cakes (sulgidduk).

There has been an increasing interest in the use of natural plant materials as alternative food preservatives. We examined the antimicrobial effects of natural plant materials used as additives against foodborne pathogens in laboratory media and Sulgidduk, oriental-style rice cakes. Cinnamon, mugwort, and garlic powder solutions (3%) were tested for their antimicrobial activities against pathogens in laboratory media. Sulgidduk prepared with different amounts of cinnamon powder (1, 3, and 6%) was inoculated with a Staphylococcus aureus or Bacillus cereus cocktail. The samples were air or vacuum packaged and stored at 22 ± 1°C for 72 h, and microbial growth was determined. Cinnamon powder showed more inhibitory properties against pathogens such as Salmonella enterica serovar Typhimurium, Escherichia coli O157:H7, Listeria monocytogenes, S. aureus, and B. cereus than did mugwort or garlic powder. The populations of S. aureus and B. cereus in Sulgidduk containing cinnamon powder were significantly lower than in the control during storage time. Different packaging methods did not result in a significant difference in pathogen growth. In a sensory evaluation, Sulgidduk containing 1 and 3% cinnamon powder did not significantly differ from the control sample in any of the attributes tested other than flavor. These results indicate that natural plant materials such as cinnamon powder could be used as food additives to improve the microbiological stability of rice cakes.

Study of determination method for heavy metals and harmful elements residues in four traditional Chinese medicine injections / 中国中药杂志

Methods for determination of heavy metals and harmful residues in traditional Chinese medicine injection were established. Graphite furnace atomic absorption spectrometry was used for determination of lead, cadmium and copper, atomic fluorescence spectrometry for arsenic and mercury. The preprocessing method was optimized. The average recoveries of 5 elements were between 91% and 112% while the precisions were less than 2%. The determination limit of lead, cadmium, copper, arsenic and mercury were 0.28, 0.014, 0.49, 0.19, 0.061 microg x L(-1), respectively. The proposed method was simple, sensitive, accurate and reliable, and could be used widely.

Studies on quality control of Xueyakang capsule / 中国中药杂志

<p><b>OBJECTIVE</b>To establish the quality control standard for Xueyakang capsule.</p><p><b>METHOD</b>Radix Rehmanniae, Cacumen Platycladi, Folium Artemisiae Argyi, Folium Nelumbinis were identified by TLC, and the content of quercitrin was determined by HPLC.</p><p><b>RESULT</b>The TLC sports developed was fairly clear, the HPLC method showed good repeatability, and the average recovery of quercitrin was 100.7% with RSD 2.0%.</p><p><b>CONCLUSION</b>The method is simple, accurate and can effectively control quality of Xueyakang capsule.</p>