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.

Determination of monosaccharide composition of polysaccharide and free monosaccharides in Cistanches Herba by ion chromatography-integral pulsed amperometry / 药学学报

Polysaccharides and free monosaccharides are important active components in Cistanches Herba, which have functions of anti-aging and immunological activity regulation. The study of monosaccharide composition in polysaccharide and free monosaccharide can lay a foundation for the study of primary structure, spatial structure of Cistanche polysaccharide and biological activity of Cistanches Herba. In this study, a method of water extraction and alcohol precipitation was used to extract Cistanche polysaccharide. Trifluoroacetic acid was selected as the hydrolytic acid for polysaccharide hydrolysis. An orthogonal experimental method is established. Three levels of acid concentration, hydrolysis temperature and hydrolysis time were selected to investigate the optimal hydrolysis condition. The optimal hydrolysis condition was 0.08 mol·L-1 trifluoroacetic acid hydrolysis at 100 ℃ for 3 h. The free monosaccharides of Cistanches Herba were extracted by water extraction. The established ion chromatogram integrated pulsed amperometry method can efficiently separate 11 monosaccharides in a short time. The method has good repeatability and high sensitivity, methodological experiment results meet the requirements of quantitative determination. It can accurately determine the monosaccharide composition of Cistanche polysaccharide and free monosaccharide content. Ion chromatography does not require derivatization operation and the pre-treatment steps are simple. This method can measure fructose, but PMP derivation-HPLC method can't. The monosaccharide composition of Cistanche polysaccharide include fucose, arabinose, rhamnose-galactose, glucose, xylose, mannose, fructose, ribose and glucuronic acid, among which the contents of glucose and fructose are relatively high. The free monosaccharides in the water extract of Cistanches Herba include glucose, fructose and mannose.

Quality Analysis and Suggestion for Ginkgo Folium Tablets and Ginkgo Folium Capsules / 中国实验方剂学杂志

Objective:To conduct quality evaluation of Ginkgo Folium preparations by analyzing the national evaluation sampling test results， analyze the quality differences， and put forward suggestions for the improvement of quality standards and market supervision. Method:The contents of total flavonol glycosides and terpene lactones in Ginkgo Folium tablets and Ginkgo Folium capsules were determined according to the methods of determination in the 2015 edition of Chinese Pharmacopoeia （the first volume）， and the contents of free flavonoids （quercetin， kaempferide and isorhamnetin） and sophoricoside in Ginkgo Folium preparations were determined according to related supplementary testing method of Ginkgo Folium tablets and Ginkgo Folium capsules issued by National Medical Products Administration. The quality differences of Ginkgo Folium preparations from different batches and different manufacturers were compared according to the contents of total flavonol glycosides， terpene lactones， free flavonoids and sophoricoside in 328 batches of Ginkgo Folium tablets and Ginkgo Folium capsules manufactured by 48 enterprises. Result:Quality of 328 batches of Ginkgo Folium tablets and Ginkgo Folium capsules was in accordance with the standard， but the contents of terpene lactones and total flavonol glycosides were all distributed in a wide range， and the quality of samples varied greatly among different enterprises. Conclusion:It is recommended that each enterprise should optimize the production process and strictly control the raw materials to ensure the consistency between different batches of samples.

Determination and Risk Assessment of Six Hepatotoxic Pyrrolizidine Alkaloids in Verbenae Herba / 中国实验方剂学杂志

Objective:To establish ultra-performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS） for simultaneous determination of six hepatotoxic pyrrolizidine alkaloids in Verbenae Herba， and to carry out preliminary risk assessment according to the research results. Method:An ACQUITY UPLC HSS T3 column （2.1 mm×100 mm， 1.8 μm） was used for analysis with 0.05% formic acid and 2.5 mmol·L^-1 ammonium formate in water （A）-0.05% formic acid and 2.5 mmol·L^-1 ammonium formate in acetonitrile （B） as mobile phase for gradient elution （0-12 min， 3%-8%B； 12-25 min， 8%-15%B； 25-26 min， 15%-3%B； 26-30 min， 3%B）， the flow rate was 0.3 mL·min^-1， the column temperature was 40 ℃， and the injection volume was 1 μL. MS system was operated by electrospray ionization （ESI） in the positive ion mode with multiple reaction monitoring mode. MS parameters of triple quadrupole and six analytes were optimized for qualitative and quantitative analysis. According to the determination results， the risk assessment was carried out by using margin of exposure （MOE） combined with transfer rate of hot water extraction. Result:Based on the instrument precision， linear range， repeatability， stability， recovery and other methodological validations， the results were in conformity with relevant standards of quantitative analysis. The linear ranges of intermedine， lycopsamine， intermedine <italic>N</italic>-oxide， lycopsamine<italic> N</italic>-oxide， echimidine<italic> N</italic>-oxide and echimidine were good （<italic>r</italic>≥0.999 0） between peak area and mass concentration in the ranges of 0.984-49.20， 0.994-49.70， 1.012-50.60， 1.032-51.60， 1.004-50.20， 1.016-50.80 µg·L^-1， respectively. The average recoveries of these six analytes were 87.2%-94.2% with relative standard deviation （RSD）<4.0%. Their MOE values were >10 000. Conclusion:The UPLC-MS/MS established in this study is stable and feasible， which can provide scientific basis for the quality control and safety evaluation of hepatotoxic pyrrolizidine alkaloids in Verbenae Herba.

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).

Simultaneous determination of six pyrrolizidine alkaloids in different parts of Emilia sonchifolia by UPLC-MS/MS / 中国中药杂志

This study aims to develop a UPLC-MS/MS method for simultaneous determination of six pyrrolizidine alkaloids(PAs)--intermedine N-oxide(ImNO), lycopsamine N-oxide(LyNO), seneciphylline(Sp), seneciphylline N-oxide(SpNO), senecionine N-oxide(SnNO), and senkirkine(Sk) in different parts of Emilia sonchifolia. UPLC conditions are as follows: ACQUITY UPLC HSS T3 column(2.1 mm×100 mm, 1.8 μm), mobile phase consisting of 0.05% formic acid and 2.5 mmol·L~(-1) ammonium formate in water(A)-0.05% formic acid and 2.5 mmol·L~(-1) ammonium formate in acetonitrile(B) for gradient elution. MS conditions are as below: electrospray ionization(ESI) in the positive ion mode, multiple reaction monitoring(MRM), and the content of the six PAs was calculated with the external standard method. The results suggested the differences in the six PAs among different parts of E. sonchifolia. Sk was detected in all the four parts, with similar content. SnNO also existed in all the four parts, but the content in roots was significantly higher than that in other parts. Sp and SpNO were found in both roots and flowers, with the content higher in the former than in the later. ImNO and LyNO were only found in leaves, and the content was low. Among the six components detected, ImNO, LyNO, and SpNO were found and determined for the first time, which enriched the toxic components and laid a scientific basis for the quality and safety evaluation of E. sonchifolia.

Quality Control of Salvianolic Acids Reference Extract / 中国实验方剂学杂志

Objective::To establish the quality control method for multi-index content determination and fingerprint of salvianolic acids. Method::Agilent ZORBAX SB-C18 (4.6 mm×250 mm, 5μm) column was adopted, with 0.1%formic acid-water as mobile phase A and 0.1%formic acid-acetonitrile as mobile phase B for gradient elution (0-30 min, 20%-21.5%B; 30-35 min, 21.5%-25%B; 35-45 min, 25%-40%B; 45-50 min, 40%-95%B). The column temperature was set at 30 ℃, the flow rate was set at 1 mL·min-1, and the detection wavelength was set at 288 nm. Relative correction factors of caffeic acid, salvianolic acid E, rosmarinic acid, lithosperic acid, salvianolic acid B and salvianolic acid Y were determined by the concentration method. The content of each indicator component of the reference extract of salvianolic acid polyphenolic acid was determined and compared with the results of the monomer reference substance by the external standard method. At the same time, the fingerprint method was established. and the similarity evaluation was carried out on 10 batches of extracts. Result::Caffeic acid, salvianolic acid E, rosmarinic acid, lithospermic acid, salvianolic acid B, and salvianolic acid Y had a good linear relationship within the respective detection mass concentration ranges (r>0.999 9). The injection precision RSD was 0.1%-1.2%, the reproducible RSD was 1.2%-1.6%, and the recovery of the six components was 82.03%-98.68%. The stability of each component in the sample solution was good within 36 h. The relative correction factors for each indicator component were determined to be caffeic acid (2.92), salvianolic acid E (1.10), rosmarinic acid (1.61), lithosperic acid (1.07), salvianolic acid B (1.00), salvianolic acid Y (0.83). The effects of different methods, concentrations, instruments, columns, wavelengths were investigated, and the measured relative correction factors were found to be suitable. The results of the calibration factor method and the monomer standard reference substance method were less different. The HPLC fingerprints of the reference extract of salvianolic acids were established, and five common characteristic peaks were determined. The chromatographic peaks were confirmed according to the reference substance. The similarity of the fingerprints of the 10 batches of extracts was higher, and the quality difference was smaller. Conclusion::The multi-index content determination method and the fingerprint method established in this study are simple, rapid, accurate and reproducible, and can be used for quality control of Salviae miltiorrhizae Radix et Rhizoma polyphenolic acid reference extract.

Determination of the bioaccessibility of cadmium and arsenic in earthworms by PBET digestion in vitro / MDCK cell model with risk assessment / 药学学报

Inductively coupled plasma mass spectrometry (ICP-MS) was used to determine the content of cadmium (Cd) and arsenic (As) in earthworms. A physiologically-based extraction test (PBET) digestion in vitro /MDCK cell model was established to investigate the bioaccessibility of Cd and As in earthworms. The hazard index (HI) method and the margin of exposure (MOE) method were used to assess the risks of the total content and the bioaccessible content of Cd and As. The results showed that the total content of Cd and As in six batches of earthworms ranged from 8.319 to 33.606 mg·kg-1 and from 0.532 to 16.412 mg·kg-1, respectively. After uptake by MDCK cells, the bioaccessibility of Cd in earthworms ranged from 10.13% to 64.16%, and the bioaccessibility of As was from 2.72% to 46.57%. The results of risk assessment showed that before uptake by MDCK cells, the MOE values of As and HI values of Cd for all batches of earthworms were greater than 1, which suggests that the risks of As are acceptable but the risks of Cd are unacceptable. After transportation by MDCK cells, except for one batch of earthworms, the HI values of Cd in the other five batches were less than 1, which suggests that the risks are at a safe level. This study provides important technical support for a more objective and scientific assessment of the health risks of heavy metals in traditional Chinese medicines, and for a more scientific and reasonable standard limit of heavy metals.

Comparison between charged aerosol detector and evaporative light scattering detector for analysis of sugar in Zhusheyong Yiqi Fumai and study on accuracy of methods / 中国中药杂志

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.

Analysis and health risk assessment, including recommendation of limits for heavy metals and harmful elements in Chinese patent medicines / 药学学报

Heavy metals and other harmful elements in traditional Chinese medicines inflict serious damage on public health. Therefore, risk assessment of Chinese raw materials has gained increasing attention. To date, few reports have been published on the health risk assessment of heavy metals and harmful elements in Chinese patent medicines. To gain a comprehensive understanding of heavy metals and other harmful elements in Chinese patent medicines and to establish proper limits, residual Pb, Cd, As, Hg, Cu and Cr in 15 054 samples of 295 drugs was analyzed with regard to distribution and variation between elements and dosage forms. In addition, in accord with procedures including hazard identification, hazard characterization, exposure assessment and risk characterization, basic procedures and specific parameters for risk assessment of heavy metals and harmful elements in Chinese patent medicines were clarified based on the health risk assessment of 14 787 samples and 276 drugs. A method and equation for establishing residual limits is proposed. The results show that content and target hazard quotients (THQs) of the investigated elements in all samples showed a skewed distribution approaching 0. Content of Pb, As, Cu, Hg, Cd or Cr in the samples exceeded 100 mg·kg-1 and the content of Pb, As, or Cu in individual samples exceeded 1 000 mg·kg-1. THQs of 586 samples and four drugs were above 1. We believe that the health risk of Hg, Pb and As in Chinese patent medicines with dosage forms of pill, capsule, tablet and powder, especially those in raw powder preparations, warrant concern.

Study on simultaneous determination of six arsenic species by HPLC-ICP-MS / 中国中药杂志

This study aims to establish a method for the determination of As B,As C,DMA,As( Ⅲ),MMA and As( Ⅴ) by using HPLC-ICP-MS. A Dioncx Ion PacTMAS7( 4 mm×250 mm) column was used for the HPLC-ICP-MS method. The mobile phase was 100 mmol·L-1 ammonium carbonate-1. 5 mmol·L-1 ammonium dibasic phosphate( gradient elution) at a flow rate of 1 m L·min-1. The injection volume was 10 μL. The linear relationships of As B,As C,DMA,As( Ⅲ),MMA,As( Ⅴ) were good with the concentration of10-500 μg·L-1. The average recovery rates( n = 6) were 105. 7%,100. 5%,102. 9%,105. 7%,100. 2%,92. 69%. The RSD were0. 50%,2. 4%,0. 93%,1. 3%,0. 89%,1. 5%. The precision and repeatability of this method were good. In this study,six forms of arsenic were separated effectively by this method. With methodological validation and sample determination,this method can be used to determine the morphological valence of arsenic in content determination.

Study on application of salvianolic acids reference extract in quality control of Salvia miltiorrhiza and salvianolic acids for injection / 中国中药杂志

The purpose of this study was to investigate the feasibility of the salvianolic acids reference extract for quality control for Salvia miltiorrhiza and salvianolic acids for injection. An Agilent ZORBAX SB-C18( 4. 6 mm×250 mm,5 μm) column was used with mobile phase consisting of 0. 1% formic acid-water and 0. 1% formic acid-acetonitrile in gradient elution procedure. The column temperature was 30 ℃; the flow rate was 1 m L·min-1; and the detection wavelength was 288 nm. The content of rosmarinic acid,lithospermic acid and salvianolic acid B in S. miltiorrhiza was determined by using the salvianolic acids reference extract as control substance. The content of caffeic acid,salvianolic acid E,rosmarinic acid,lithospermic acid,salvianolic acid B,and salvianolic acid Y in the salvianolic acids for injection was also determined. The linear relationship between chemicals was good( r>0. 998 9),and the injection precision RSD was 0. 30%-0. 90%. The sexual RSD is between 1. 4% and 3. 0%,and the RSD of the reproducibility of the extract is between 2. 1% and 5. 2%. The recovery rate of the three components in S. miltiorrhiza was 96. 80%-99. 20%,and the recovery rate of the six components in salvianolic acids for injection was 88. 90%-107. 5%. The solution of S. miltiorrhiza and salvianolic acids for injection were stable within 48 h. A total of 8 batches of S. miltiorrhiza and injection were determined by the reference extract,and the difference was smaller than that measured by the monomer control. This study preliminarily verified that the salvianolic acids reference extract can be used as a substitute for the monomer control for the quality control of S. miltiorrhiza and salvianolic acids for injection.

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.

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.

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 forbidden and restricted pesticides in Angelicae Sinensis Radix / 中国中药杂志

The present study is to establish a method for simultaneous determination of 50 kinds of pesticides in Angelicae Sinensis Radix by using liquid chromatography tandem mass spectrometry. The forbidden,restricted and customary pesticides were picked out as detecting indexes according to the principals of risk management. The factors affecting the extraction,purification,and detection were optimized,and the final condition was established as follows: the samples were extracted with acetonitrile. The separation of target compounds were performed by liquid column,and quantitative analysis was carried out by LC-MS/MS with MRM model. The calibration curves were linear in the range of 1-100 μg·L~(-1) with correction coefficients of greater than 0. 990. The recoveries of more than 93. 9%pesticides were ranged from 60% to 140% at three spiked levels. The detecting indexes in the method cover most forbidden and restricted pesticides,which is meaningful for the safety supervision of the Angelicae Sinensis Radix. With the advantage of rapidness and accuracy,this method can be used for routine determination of multi-pesticides in Angelicae Sinensis Radix.

Relative molecular weight determination of astragalus polysaccharides for injection / 药学学报

To determine relative molecular weight of astragalus polysaccharides (APs), we used Shodex GS620 gel permeation chromatographic column and differential refraction detector (GPC-RI) with dextran as a reference. Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF-MS) and GPC combined with multi-angle laser light scattering detection (GPC-MALLS) were also used．GPC-RI measure showed four peaks of APs, with the Mw of 1 380 000, 231 000, 18 000, and 480, respectively. Three main peaks were found by GPC-RI-MALLS with the Mw as 1 148 000, 180 000, and 43 000, respectively. Strong signals in 155 000 and 18 000 were detected by MALDI-TOF-MS, which also indicated the sugar moieties of the APs as hexoses. From our study, we found that the GPC-RI method with universal correction is most suitable for Mw determination of the APs. Nevertheless, the three methods should be combined and contrasted with each other to obtain accurate information in research of polysaccharides from Chinese medicine.

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.

Dissipation dynamics of spirodiclofen in wolfberry fruit / 中国中药杂志

The dissipation of spirodiclofen in fresh fruit and dry fruit of wolfberry was detected in this study to provide a reference for its safe application.According to Pesticide Residue Test Criteria of China, the open-field experiment was conducted in Zhongning courty of Ningxia province, and the dissipation of spirodiclofen was studied by acetonitrile extraction and HPLC-MS/MS detection. The results showed that the half-lives of spirodiclofen in fresh wolfberry fruit and dry wolfberry fruit were 6.9-11.2 days and 8.5-10.4 days, respectively. Spirodiclofen belongs to the easily degradable pesticide type. According to the maximum residue limits (0.5 mg•kg⁻¹) of spirodiclofen of EU for wolfberry, after recommended dosage being sprayed for once, fresh wolfberry fruit was safe to eat after 5 days, and dry wolfberry fruit was safe to eat after 21 days.