The objective of this study was to evaluate the relationship between beta-galactosidase activity in urine, in serum and urinary N-acetyl-beta-glucosarminidase activity as an early indicator of renal effect and mercurT concentration in urine and blood, reflecting the intensity of exposure to or the amount of body burden of mercury. This study was carried out among 70 workers exposed to mercury vapor and 63 non-exposed workers as a reference. The results were as follows ; 1. The mean concentration of urinary mercury (43.5 microgram/1) in exposed subjects was about nine times higher than that of non-exposed subjects, but the mean values of blood mercury were not different from each other 2. The mean values of beta-galactosidase activity in urine (119.7micromoleMU/h/g creatinine) and in blood (73.7 moIMU/H/l) of mercury-exposed subjects were significantly higher than those of non-exposed subjects. 3. In mercury-exposed subjects, beta-galactosidase activities in urine (r=0.38, p<0.01) and in serum (r=0.26, p<0.05) were correlated to urinary mercury concentration, but not to blood mercury concentration. The urinary excretion of beta-galactosidase activity was closely associated with urinary mercury concentration in the result of the multiple regression analysis. 4. The urinary beta-galactosidase activity in exposed subjects increased as the urinary mercury increased, and in the exposed subjects with more than 50microgram/1 of urinary mercury was highly related to urinary beta-galactosidase activity(r=0.47, p<0.05). 5. Among exposed subjects with more than 50microgram/l of urinary mercury, 20.0% of them showed abnormal value of urinary beta-galactosidase activity.
beta-Galactosidase* ; Body Burden

OBJECTIVETo determine organochlorine pesticide residue in 9 Chinese herbs.

METHODSThe organochlorine pesticides were extracted from the herbs with mixed solvents of n-hexane and acetone by a solid-phase extraction cartridge Florisil. Capillary gas chromatography was used to separate the samples.

RESULTSGood linearities were obtained for 11 organochlorine pesticides. The average recoveries at two concentration levels ranged from 79.9% to 89.0%,and from 86.3% to 104.8%, with relative standard deviations of 1.8% to 7.1%, respectively and detection limit of 2 g/kg. The residues of the organic pesticides exceeded national standard in Pogostemon cablin and Panax notoginseng.

CONCLUSIONCapillary gas chromatography combined with electron capture detection provides a practical means for detecting organic pesticide residue in Chinese herbal medicines, and the limits of pesticide residues should be formulated in Chinese pharmacopoeia.

OBJECTIVETo determine the pesticide residues in Shengmaiyin.

METHODThe residues were simultaneously identified and quantified by capillary gas chromatography. The capillary column was OV-1701(0. 32 mm x 30 m, 0.5 microm), splitless injection and Agilent 63Ni electron capture detector ECD were adopted. The carrier gas were high-pure nitrogen, the flow rate were 60 mL x min(-1), the injector temperature was 260 degrees C, and the detector temperature was 300 degrees C.

RESULTIt showed a good linear relationship between peak area and pesticide concentration for 11 kinds of pesticides in the detection concentration range. All correlation coefficients were higher than 0.996 2. The average recovery was 83.1% -114.7%.

CONCLUSIONA simple and efficient monitoring method of pesticide residues is established which provides the foundation for the safe use and analysis of Shengmaiyin.

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.
China ; Drug Contamination ; prevention & control ; Pesticide Residues ; analysis ; Plants, Medicinal ; chemistry ; Quality Control

The residue of the pesticides is closely related to the quality and safety of traditional Chinese medicines(TCMs) and has attracted widespread attention at home and abroad.This article analyzed the current status of pesticide residues in TCMs by summarizing the research results of recent years.At the same time,the methods for the detection of pesticide residues in TCMs were summarized,and the domestic and foreign pesticide residue limit standards for TCMs were compared,intending to provide reference and basis for the detection and control of pesticide residues in TCMs.
Drug Contamination ; Drugs, Chinese Herbal ; analysis ; Medicine, Chinese Traditional ; Pesticide Residues ; analysis ; Research

The present paper outlined pesticide registration status for traditional Chinese medicines (TCMs) and summarized the characteristics of pesticide contamination in different regions of some widely used TCMs by retrieving last 10 years' literatures. At present, the problems of pesticide residues for TCM include less pesticide registrations, widespread high-residue organochlorine pesticides contamination, pesticide abuse, irregular GAP bases and imperfect pesticide limit standards, etc. According to the current situation, we should adopt some control measures to strengthen the quality control of TCMs so as to ensure the safety of TCMs and related products.
Animals ; China ; Drug Contamination ; prevention & control ; statistics & numerical data ; Humans ; Medicine, Chinese Traditional ; methods ; Pesticide Residues ; analysis ; Registries

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.
Chromatography, Gas ; Chromatography, Liquid ; Drug Contamination ; Drugs, Chinese Herbal ; analysis ; Pesticide Residues ; analysis ; Quality Control ; Tandem Mass Spectrometry

In recent years, the quality and safety problems have been limiting the internationalization of Chinese medicine. The pollutants in Chinese medicine, particularly the exogenous harmful pollutants mainly including mycotoxins, pesticide residues, heavy metals, harmful elements, and sulfur dioxide, are of high risks for people. Therefore, the World Health Organization(WHO) and relevant national organizations have clearly defined the maximum residue limits(MRLs) of such pollutants. Chinese Pharmacopoeia(2020 edition, volume Ⅳ) also demonstrates the detection methods, MRLs and preliminary risk assessment methods for four typical exogenous harmful pollutants in Chinese medicine. Therefore, continuous optimization of the health risk assessment system can further help further raise the quality and safety of Chinese medicine. This paper reviews the research on the health risk assessment of four typical exogenous harmful pollutants in Chinese medicine and discusses the problems of and challenges for the assessment system, which is expected to lay a scientific basis for the establishment of the risk warning mode and response measures suitable for specific types of Chinese medicine.
Drug Contamination ; Drugs, Chinese Herbal/analysis* ; Environmental Pollutants/analysis* ; Humans ; Medicine, Chinese Traditional ; Pesticide Residues/analysis* ; Risk Assessment

In order to study the pesticide residues of the medicinal Crataegi Fructus,this study aims to establish an analysis method for pesticide residues( mainly containing insecticides and fungicides) suitable for the actual situation of medicinal Crataegi Fructus based on the survey of the pesticides of the Crataegi Fructus base,combined with the blind screening results of the LC-ESI-MS/MS pesticide screening platform established by the research team in the early stage. Then,the pesticide residues in medicinal Crataegi Fructus from Shandong,Hebei,Henan,Shanxi,and Liaoning( main cultivation areas) were analyzed. The samples were pretreated by the modified Qu ECh ERS method,i.e.,extracted with acetonitrile-water( 9 ∶1),purified by PSA,C_(18),GCB,silica gel. The detection of pesticides was performed by LC-MS/MS. The ion source was ESI with positive scanning mode,and the linearity of 11 kinds of pesticides in the range of 5-300 μg·kg~(-1) was acceptable( R~2>0. 996 9). All the recoveries of pesticides were within 70. 02%~(-1)12. 0% in the low,medium and high levels,with RSD≤17%. The results showed that the detection rate of carbendazim,chlorpyrifos and difenoconazole is 79%,82%,56%,respectively. Besides,the prohibition pesticide carbofuran were detected in some of the batches,indicating the security risk. This study provides methodological references and basic data for risk assessment of Crataegi Fructus and government regulation.
Chromatography, Liquid ; Crataegus/chemistry* ; Drug Contamination ; Drugs, Chinese Herbal/analysis* ; Pesticide Residues/analysis* ; Surveys and Questionnaires ; Tandem Mass Spectrometry

This study proposed a quantitative method for 34 pesticides including organochlorine,organophosphorus and pyrethroids in Glycyrrhizae Radix et Rhizoma herbs and medicinal slices,and analyzed the pesticide residues of collected Glycyrrhizae Radix et Rhizoma samples from different regions. With acetonitrile extraction and optimized Qu Ech ERS purification,the 32 batches of Glycyrrhizae Radix et Rhizoma herbs and medicinal slices were analyzed by matrix matching standard curve quantitative analysis under GC-MS/MS multi-response monitoring( MRM) mode. This study investigated the pretreatment of Glycyrrhizae Radix et Rhizoma samples based on the Qu Ech ERS method of Chinese Pharmacopoeia( 2015 edition,4),and the result showed that the recoveries of some pesticide was low and pigment has a strong interference in analysis,which result in worse purification effect. Therefore,this paper further optimized the Qu Ech ERS method and corrected the matrix matching standard curve method,and compensated the qualitative and quantitative effects of matrix effects on the detected target compounds in Glycyrrhizae Radix et Rhizoma. The results showed that 34 kinds of pesticide had good linear( R~2 of 0. 996 4 or higher) within a covering 0. 01-0. 2 mg·kg~(-1) concentration range. The limits of quantitation are less than 0. 01 mg·kg~(-1). This method was further applied to the simultaneous determination of 34 pesticide residues of typical organochlorine,organophosphorus and pyrethroids in 32 batches of Glycyrrhizae Radix et Rhizoma herbs and medicinal slices. Six batches containing beta-endosulfan,thiosulphate,o,p'-DDD and thrta-cypermethrin were detected,but none of them exceeded the limit of pesticide residues stipulated in the Chinese Pharmacopoeia and the EU Pharmacopoeia. This study indicates that the established method is rapid,convenient,accurate,and sensitive,which provides a rapid and efficient method for the simultaneous determination of typical organochlorine,organophosphorus and pyrethroids in Glycyrrhizae Radix et Rhizoma.
Drug Contamination ; Drugs, Chinese Herbal/analysis* ; Gas Chromatography-Mass Spectrometry ; Glycyrrhiza/chemistry* ; Pesticide Residues/analysis* ; Rhizome ; Tandem Mass Spectrometry