A rapid and accurate method of quantifying heavy metal pollution in commercial traditional Chinese medicines (TCMs) is described. The method uses modified wet digestion for sample preparation and atomic absorption spectrophotometry for detecting the content of copper (Cu), cadmium (Cd), arsenic (As), lead (Pb) and mercury (Hg). The determination limits of the method were 0.001, 0.002, 0.001, 0.001 and 0.001 mg/kg for Cu, Cd, As, Pb and Hg, respectively. The method was applied to the quantification of heavy metal pollution in 50 different commercial TCMs in a total of 250 samples. Heavy metal contents in the samples investigated were found at different levels. The level of As did not exceed the legal limit stated in the China pharmacopoeia 2010, whereas Cu, Cd, Pb and Hg were above permitted levels in some samples.

A total of 110 commercially available samples of manufactured food products including bread, oat, barley, maize, corn, wheat, grape, soluble coffee, soya bean, red wine, and baby food were randomly collected in the northeast of China during the first six months of 2010. Samples were analyzed for the presence of ochratoxin A (OTA) using immunoaffinity column (IAC) clean-up and high-performance liquid chromatography with fluorescence detection (HPLC-FD) and confirmed with LC–ESI–MS/MS. The range of average OTA recoveries was 78.3–103.3% at three spiked levels. The relative standard deviations (RSDs) of recoveries range of 2.1–4.3%. OTA were detected in 13 samples, which were below the maximum allowable limit established by the European Community. The results of this study suggest that those manufactured food products consumed in China present no risk by human exposure to OTA through their consumption.

Many natural compounds of biological and pharmacological interest are asymmetric and show optical activities; for example, optical isomers of ephedrine produce different amphetamine-like stimulus effects, and (S)-(-)-alpha-ionone (woody-like taste) and (R)-(-)-alpha-ionone (violet taste) possess different olfactory properties, etc. Consequently, the need for enantiomerically pure natural compounds is a growing concern for active research in pharmacology, biochemistry, and the quality control of chiral natural compounds. Different kinds of chiral selectors including crown ether, macrocyclic antibiotics, cellulose, and cyclodextrins (CDs) have been investigated to resolve optical natural products. Among them, cyclodextrins and their derivatives are the most frequently employed chiral selectors and are used as stationary phase or additives in the separation of natural products for their powerful ability in chiral resolution and the various available products in the market. This review first summarizes the utility of CDs and their derivatives as stationary or additives in the chiral resolution of natural products, typically flavanones, alkaloids, lignans, coumarins, terpenoids, amino acids, peptides, etc. In addition, analytical techniques of gas chromatography (GC), high-performance liquid chromatography (HPLC), capillary electrophoresis (CE), and capillary zone electrophoresis (CZE) applied in separation of optical natural products using CDs or their derivatives as chiral selectors are also summarized.

Toxic metal contamination was investigated in Artemisia annua L. herbal preparations from different commercial sources in China. Measurable amounts of copper (Cu), lead (Pb), arsenic (As), mercury (Hg), cadmium (Cd), chromium (Cr), manganese (Mn), nickel (Ni) and aluminium (Al) were detected in commercial dried Artemisia annua L., Massa Medicata Fermentata (Shenqu), Semen Sojae Praeparatum, medicated leaven (Jianqu) and an oral dose of Zhongganling-pian by inductively coupled plasma optical emission spectrometry (ICP-OES) and atomic fluorescence spectrometry (AFS). A total of 69 samples were collected from different sources in the Chinese market. Toxic metals contents in the investigated samples were found at different levels. Results showed that 94.20, 100, 97.10, 91.30 and 94.20% of the products fully complied with the quality requirement for traditional medicines in China pertaining to Cu, Pb, As, Hg and Cd, respectively. Although toxic metal concentrations measured in this study do not pose a serious health risk, they do affect the quality of herbal preparations. Moreover, on the basis of the results obtained in the present work, it is concluded that the present techniques are suitable for the routine determination of toxic metals concentration in various pharmaceutical dosage forms.

The Quick Easy Cheap Effective Rugged and Safe multiresidue method (QuEChERS) has been validated for the extraction of 15 organochlorine pesticides (OCPs) in completely different matrices of traditional Chinese medicine (TCM). The method employed a rapid, simple and cost-effective procedure. The spiking levels for the recovery experiments were 0.1, 0.5 and 2.0mgkg−1. Mean recoveries mostly ranged between 76.0% and 114.0% (96.0% on average), and relative standard deviations (RSD) were generally below 10% (4.72% on average). Based on these results, the methodology has been proven to be highly efficient and robust and thus suitable for monitoring the MRL compliance of a wide range of commodity. The contamination status of 15 OCPs on 80 different TCMs marketed in China, and a total of 400 samples were also performed using a previously validated method. 15 OCPs were benzene hexachloride (BHC, including α-BHC, β-BHC, γ-BHC, δ-BHC), hexachlorobenzene, heptachlor, heptachlor epoxide, aldrin, p, p′-DDE, p, p′-DDD, o, p′-DDT, p, p′-DDT, mirex, endrin, dieldrin. This study indicates that the proposed method is useful for analyzing OCPs in TCM.

LC–ELSD has been applied for the determination of T-2 and HT-2 toxins in Traditional Chinese Medicine (TCM) marketed in China. For sample preparation, two clean-up procedures were developed using Florisil and MycoSep227 for solid-phase extraction. Limits of detection (10 ng g−1) as well as recoveries are described. A total of 138 samples of 46 commercially available TCM samples was analyzed; only one sample was determined to contain T-2 at a level of 64.0 ng g−1, and positive results were further confirmed by LC–ESI–MS–MS.

Zearalenone (ZEA) is one of the most widely distributed mycotoxins produced by Fusarium species, responsible for important diseases of barley. The present work shows the results of a rapid and accurate method to quantify ZEA in barley. The method uses the Quick Easy Cheap Effective Rugged and Safe method (QuEChERS) for purification and high-performance liquid chromatography coupled with an evaporative laser scattering detector (HPLC–ELSD) for detection and quantification of the toxin. Barley samples were extracted with methanol and used acetonitrile–water–methanol (46:46:8, v/v) as mobile phase. Average recoveries of ZEA from barley spiked at levels of 0.1–10μg/g ranged from 83.0% to 91.5%, with relative standard deviations of <6%. The detection limit was 1.56ng/g based on a signal-to-noise ratio of 3:1. Using this method, we have analysed a total of 175 samples of 35 functional food marketed in China. The results showed that the overall level of ZEA contamination was relatively low (5.14%) and the presence of ZEA was found in nine samples at concentrations ranging from 11.09 to 26.54ng/g.

A simple and rapid method was developed for determining nine pesticide residues in fifty traditional Chinese medicine.Pesticides were extracted with mixed solvents of acetonitrile,water and 1% acidum aceticum(95:4:1,V/V/V).Extracts were cleaned-up by QuEChERS(Quick,Easy,Cheap,Effective,Rugged and Safe) pesticide multiresidue method,and then detected by gas chromatography with electron capture detection.Good linearity was obtained in the concentration range of 1.0～100 ng/mL.Average recoveries of 9 pesticides at three concentration levels were in the ranges of 76.0%～114.0%,86.1%～95.7% and 82.8%～104.6%,respectively.The limits of detection of 9 pesticides were in the ranges of 0.4～1.5 μg/kg.The method is easy and low-cost.

目的 建立免疫亲合柱(IAC)-高效液相色谱.蒸发光散射(HPLC-ELSD)检测常用中药中赭曲霉毒素(OTA)的方法.方法 样品经甲醇-水(85:15)振荡提取后,通过IAC净化洗脱,HPLC分离定量.结果 OTA在2～200 ng/mL,呈良好的线性关系,r为0.998 9;OTA的最低检出限为0.5 ng/g;回收率为89.8%～94.6%,RSD为3.1%～6.9%.结论 建立的IAC-HPLC方法检测常用中药中OTA无干扰性杂峰,结果准确可靠.

就硫黄在医药及农业等领域的应用研究进行了综述,并对其今后研究方向进行了展望.

The study aimed to establish the method for determining simultaneously deoxynivalenol(DON) and nivalenol (NIV) in Radix Panacis Quinquefolii.The method is to extract the sample with a mixture of acetonitrile-water (75:25).The extract was purified by multifunctional cleanup column.DON and NIV were then separated and determined by reversed-phase HPLC with C_(18) column and a mixture of water-acetonitrile(80:20) as mobile phase.The results showed that the average recoveries of DON and NIV from the Radix Panacis Quinquefolii spiked at levels of 0.15～20μg·g~(-1) ranged from 86.4%～91.5%,with the relative standard deviation less than 8%.The detection limits for DON and NIV were 15 and 10 ng·g~(-1)(S/N=3),respectively.The conclusion is that the content of DON and NIV in the Radix Panacis Quinquefolii were determined for the first time.The established method can be used in determining the contents of multiple DON and NIV in the Radix Panacis Quinquefolii simultaneously.

A fast pesticide multiresidue analysis method using gas chromatography coupled with electron capture detector was investigated for the simultaneous determination of 15 organochlorine pesticides (OCPs) in American ginseng (Panax quinquefolium L.). Samples were extracted with acetic acid–water–acetonitrile (1:5:94, v/v) and cleaned up by the Quick Easy Cheap Effective Rugged and Safe multiresidue method (QuEChERS). The linearity for 15 OCPs, in the working standard solutions of seven concentration levels between 1 and 100 ng/ml, varied from 0.9990 to 0.9999. Recoveries at concentrations between 0.1 and 2 μg/g ranged from 81.4 to 95.2%, with precision, which was expressed as relative standard deviation (RSD), at values lower than 8.0%. The proposed method was applied to the determination of pesticide levels from 60 samples, taken from six different areas. Among a total of 60 samples, 15.0% (9 samples) contained at least one of the 15 pesticides. The 15 OCPs were benzene hexachloride (BHC, including α-BHC, β-BHC, γ-BHC, δ-BHC), hexachlorobenzene, heptachlor, heptachlor epoxide, aldrin, p,p′-DDE, p,p′-DDD, o,p′-DDT, p,p′-DDT, mirex, endrin and dieldrin. This study indicates that the proposed method is useful for analyzing OCPs in American ginseng.

The multidimensional gas chromatography (MDGC) is getting affractive due to its advantages,such as high speed and efficiency,and easy combination with other technologies.This review summarized the recent developments of MDGC,and its applications in traditional Chinese medicine study.In addition,the prospect and further developments of MDGC were discussed.

A total of 125 wine and beer samples, including 42 white, 63 red wine and 20 beer samples, originating from several areas of China were analyzed for ochratoxin A (OTA). An analytical method based on immunoaffinity column (IAC) for clean-up and high performance liquid chromatography with fluorescence detection (HPLC-FD) was used to determine OTA. Positive results were further confirmed by LC-MS-MS. OTA was detected in 22 (17.6%) samples at levels of 0.02-1.18 ng/ml, which were below the EU maximum limit. The mean OTA concentration in red wine was slightly higher than in white wine. This study showed that OTA occurs in wine and beer in China but at levels that pose no danger of significant human exposure to OTA from this source.

多维高效液相色谱以其快速、高效、自动化程度以及易与质谱等其他技术联用等优势成为研究应用的热点。对近年来多维液相色谱技术及其在中药研究中的应用进行了综述,并对多维液相色谱的发展趋势和前景进行了展望。

对淫羊藿抗骨质疏松症的相关研究近况进行综述,阐述淫羊藿的抗骨质疏松症作用及其作用机制,为中药抗骨质疏松症的研究提供理论基础。

OBJECTIVE: To study the effects of carbendazol on the contents of indigotin and indirubin in Isatidis indigotica.METHODS:Three trial groups were designed in a field experiment,and the samples were collected in 9 different periods.The contents of indigotin and indirubin in Isatidis indigotica were determined by HPLC.RESULTS:The contents of indirubin and indigotin in high and low concentrations of carbendazim-treated groups were lower than in blank control group.CONCLUSION:At a certain concentration,carbendazol can decrease the contents of indigotin and indirubin in Isatidis indigotica.

用丙酮提取大青叶样品中的多菌灵,采用液-液萃取法进行样品前处理,采用高效液相色谱法测定了样品中多菌灵的残留量.结果表明,方法的最低检测量多菌灵为0.149 44 ng,样品为2.102 44 ng.添加3个水平的多菌灵对照品溶液,回收率范围在72.27%～89.57%之间,符合农药残留分析要求.田间降解动态试验结果表明,高浓度多菌灵在大青叶中降解半衰期为2.92 d,低浓度多菌灵在大青叶中降解半衰期为2.74 d.施用高、低浓度多菌灵后,大青叶采收距最后一次施药的安全间隔期推荐分别为21.22 d、17.38 d.

对镰刀菌毒素物理过程、化学过程、生物过程.分了生物及植物育种过程在内的镰刀菌毒脱毒技术研究进展进行综述,并对其在药用植物中的应用前景进行展望.

Objective:To detect the content of polysaccharides in the health drink.Methods:Phenylhydrate sulfuric acid method was used.Results:The maximum absorption wavelength was 485 nm.Linear range was 0～0.1 mg (Y=4.628 2X-0.0066,r=0.9995).The polysaccharide content was 44.85mg·(100mL)~(-1).The average recov- ery was 97.57% and RSD was 2.97%.Conclusion:Improved Phenylhydrate sulfuric acid method was simple and ac- curacy.It can be used to determine polysaccharides in the health drink.