A solid phase extraction (SPE) and GC-ECD for multi-residues determination of 14 organo-chlorinated pesticides (OCPs) in radix Pseudo-ginseng were introduced. Using n-hexane as extracting solvent and silica gel for clean up of sample extract, with GC-ECD analysis, good separation of 14 OCPs and carbophenothion(IS) was achieved on capillary column coated with poly(5% diphenyl) siloxane. Experiments showed that n-hexane is adequate as extracting solvent(percentage of recovery70% for 13 in total 14 analyses), the LOD was about 0.35 to 1.6 ppb for blank sample spiked with standards. The method has been carried out on 7 samples collected from market for preliminary investigation of its actual OCPs residues. For 14 OCPs being analysed, results showed that all samples to be examined are complied with requirements of MRL in USP 24 or in Eur. P97.We may conclude that those samples were cultivated in less contaminated soils or none of 14 OCPs was still in illegal use
Panax ; chemistry ; Drug Residues ; drugs

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.

Chromatography, Gas ; methods ; Drug Contamination ; prevention & control ; Drugs, Chinese Herbal ; chemistry ; Pesticide Residues ; analysis ; Reproducibility of Results

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.

Chromatography, Gas ; Drug Contamination ; Drugs, Chinese Herbal ; chemistry ; Hydrocarbons, Chlorinated ; analysis ; Pesticide Residues ; analysis

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

OBJECTIVETaking Caulis Aristolochiae Manshuriensis (Guanmutong in Chinese, derived from the stem of Aristolochia manshuriensis) as an example, to study the affection of different preparations on the content of toxic constituents in traditional Chinese medicines.

METHODThe separation was performed on a zorbax SB-C18 column with mobile phase of acetonitrile-3.7 mmol x L(-1) phosphoric acid buffer, detected at 260 nm.

RESULTThe extraction percentage of aristolochic acids I, II and IV a in water extraction (1 h x 2) of Guanmutong were 53.4%, 75.5% and 61.9%, respectively; the remaining quantity of aristolochic acids I, II and IVa in the dregs of the decoction were 22.3%, 15.7% and 30.3%, respectively; Aristolochic acid I was still main substance among these aristolohic acids in the decoction of Guanmutong.

CONCLUSIONThe content of toxic constituents of the traditional Chinese medicines varies evidently with different preparations of Guanmutong. So the preparation methods of traditional Chinese medicines should be suitably selected according to characteristics of the toxic constituents so as to lessen the body damages of human.

Aristolochia ; chemistry ; Aristolochic Acids ; analysis ; Drug Residues ; chemistry ; Drugs, Chinese Herbal ; administration & dosage ; chemistry ; isolation & purification ; Pharmaceutical Solutions ; chemistry ; Plants, Medicinal ; chemistry ; Powders ; chemistry

OBJECTIVETo study eleven organophosphorus insecticides residuals in four kinds of Chinese crude drugs.

METHODThe organophosphorus insecticides were extracted with dichloromethane and cleaned-up with a mixture of Celite 545-activated carbon. The extracts were analyzed by gas chromatography equipped with a flame photometric detector (FPD).

RESULTAnalysis of fortified Chinese crude drug showed that the average recoveries ranged from 77.5% -112.3% at three different levels, the RSDs were below 10% (n = 4). Trace organophosphorous pesticide residues were found in samples of Rhizoma Atractylodis Macrocephalae and Flos Chrysanthemi.

CONCLUSIONA method was established for determination multi-residues in Rhizma Atractylodis Macrocephalae, Radix Curcumae, Bulbus Fritillariae Thunbergii and Flos Chrysanthemi. It provides a method for the risk assessment of organophosphorous pesticide in Chinese crude drugs.

Atractylodes ; chemistry ; Chromatography, Gas ; Chrysanthemum ; chemistry ; Curcuma ; chemistry ; Drug Contamination ; Drugs, Chinese Herbal ; chemistry ; Fritillaria ; chemistry ; Organophosphorus Compounds ; analysis ; Pesticide Residues ; analysis ; Plants, Medicinal ; chemistry

OBJECTIVETo establish a high-performance liquid chromatography-mass spectrometry (HPLC-MS/MS) method for detection of nine penicillin residues in milk.

METHODSThe samples were precipitated with acetonitrile and degreased with n-hexane for pre-processing. The chromatography was performed by reversed-phase HPLC in a C₁₈ column and eluted gradiently on line for 11 min. The mobile phases were water with formic acid (pH 3.1) and acetonitrile-water with formic acid (pH 3.1). By optimizing the mass condition, the method was operated by multiple-reaction monitoring (MRM) and quantitated by external standard calibration.

RESULTSThe standard curves were linear in concentration range of 0.4 approximately 400 μg/L and all nine penicillins showed a good linear relationship in the milk matrix (r>0.990). The detection limit of the method was from 0.1 to 0.8 μg/L while the limit of quantification was from 0.3 to 2.6 μg/L. The average recoveries were higher than 80%. The within-day precisions were less than 8.5%.

CONCLUSIONThe established method is convenient, rapid and accurate and meets the requirement of monitoring penicillin residues in milk.

Animals ; Chromatography, High Pressure Liquid ; methods ; Drug Residues ; analysis ; Milk ; chemistry ; Penicillins ; analysis ; Tandem Mass Spectrometry ; methods

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

A Bacillus stearothermophilus var. calidolactis C953 tube test was evaluated for its ability in detecting the residue of selected anticoccidial drugs in poultry, specically sulfamethazine, furazolidone, and amprolium. Various concentrations of each drug were injected into chicken liver and kidney tissues and these tissues were tested to determine the drug detection limits for each drug. The detection limit was defined as the drug concentration at which 95% of the test results were interpreted as positive. The limits of detection in liver tissue were 0.35 microgram/ml for furazolidone, 0.70 microgram/ml for sulfamethazine and 7.80 microgram/ ml for amprolium. In kidney tissues, they were 0.30 microgram/ml for furazolidone, 0.54 microgram/ml for sulfamethazine, and 7.6 microgram/ml for amprolium. It was concluded that this tube test could be used to screen for the residue of these three drugs in poultry.
Amprolium/analysis ; Animals ; Bacillus stearothermophilus/*drug effects ; Coccidiostats/*analysis ; Drug Residues/*analysis ; Furazolidone/analysis ; Kidney/chemistry ; Liver/chemistry ; *Poultry ; Sulfamethazine/analysis