Wild edible mushrooms can accumulate significantly elevated levels of mercury from the surrounding environment, which could be harmful to consumers’ health. Speciation analysis of mercury in wild edible mushrooms aids in understanding the human exposure to these toxic compounds. In this study, we developed a high-performance liquid chromatography hyphenated to inductively coupled plasma mass spectrometry (HPLC-ICP-MS) method for the simultaneous determination of inorganic mercury (Hg(II)), methylmercury (MeHg), ethylmercury (EtHg), and phenylmercury (PhHg) in wild edible mushrooms. A rapid separation of four target mercury species was achieved within 11 min by a C8 column without utilizing high proportion of organic phase in HPLC. The parameters affecting the extraction efficiency of mercury in samples have been investigated. The proposed method showed good linearity within 0–50 μg/L with the detection and quantification limits of 0.6–4.5 μg/kg (S/N = 3), and 2.0–15 μg/kg (S/N = 10), respectively. This proposed method was successfully applied to the mercury speciation analysis in 7 varieties (95 samples) of wild edible mushrooms. The results indicated that in most mushroom samples, mercury mainly occurred as inorganic mercury. But there were two Tricholoma matsutakes, one contained 0.14 mg/kg of methylmercury, another contained 1.05 mg/kg of phenylmercury, which were higher than the maximum allowable content of total mercury in edible mushrooms in China.

建立同时测定果蔬中抑食肼、甲氧虫酰肼、环虫酰肼、虫酰肼4种双酰肼类农药残留的超高效液相色谱法.方法用含1％氨水的甲醇溶液对样品进行提取,提取液经过乙二胺-N-丙基硅烷(PSA)和十八烷基硅烷键合相(C18)基质分散净化后,采用Agilent RRHD SB-C18柱(2.1 mm ×50 mm,1.8 μm)分离,Agilent 1290 Infinity超高效液相色谱仪DAD检测器进行检测.可在4 min内完成对4种双酰肼类农药的检测,且在0.05～10 μg/mL范围内具有良好的线性关系,相关系数R在0.998 6～0.999 8之间,方法定量为12.94～17.32 μg/kg,方法检出限为3.882～5.196 μg/kg.在0.05～2.5 mg/kg范围内,平均加标回收率为72.4％～100.4％,相对标准偏差为2.1％～6.1％.该方法灵敏度高、选择性好、操作简单,适用于果蔬中4种双酰肼类农药残留的同时快速分析.

目的 建立同时测定饮用水中5种消毒副产物(ClO2-、ClO3-、BrO3-、二氯乙酸、三氯乙酸)的离子色谱测定方法.方法 采用英蓝超滤在线样品前处理装置直接大体积进样,进样体积为100μl,Metrohm-940型离子色谱仪,电导检测器测定.流动相为乙腈-3.6 mmol/L碳酸钠溶液(10∶90,V/V);流速为0.7 ml/min.结果 五种消毒副产物线性相关系数≥0.9995,加标回收率为83.3％～116.7％,RSD≤5％,方法的定量限为:ClO2-:0.10 mg/L、BrO3-:0.002 mg/L、ClO3-:0.10 mg/L、二氯乙酸:0.010 mg/L、三氯乙酸:0.020 mg/L.结论 该法准确度好,灵敏度高,简单方便,适用于水中5种消毒副产物的同时测定.

建立松茸中钾、钠、铝、锰、锌、铜、铁、钙、镁的微波消解-电感耦合等离子体发射光谱法测定方法.样品采用3 mL硝酸和2 mL过氧化氢作为消化液,微波消解后,用电感耦合等离子体发射光谱法进行测定.结果表明:各元素线性范围为钠0～2.00μg/mL,钾0～100.00μg/mL,铝、锰、锌、铜、铁、钙、镁均为0～5.00μg/mL,平均回收率在94.14％～102.30％ 之间,相对标准偏差(RSD)为0.23％～3.21％ 范围,检出限为0.33～5.25 mg/kg,定量限为1.10～17.50 mg/kg.测得四川省6个主产区松茸中钾、钠、铝、锰、锌、铜、铁、钙、镁的含量范围分别为21～35 g/kg、42.1～117 mg/kg,183～1210 mg/kg,10.2～91.8 mg/kg,23.1～69.5 mg/kg,21.6～37.2 mg/kg,159～1174 mg/kg,51.2～349 mg/kg,441～740 mg/kg.该方法简便、快速、准确,适用于松茸中上述9种元素的同时测定.

Owing to the strong concentration and biotransformation of arsenic, the influence of some edible mushrooms on human health has attracted widespread attention. The toxicity of arsenic greatly depends on its species, so the speciation analysis of arsenic is of critical importance. The aim of the present review is to highlight recent advances in arsenic speciation analysis in edible mushrooms. We summarized the contents and distribution of arsenic species in some edible mushrooms, the methods of sample preparation, and the techniques for their identification and quantification. Stability of the arsenic species during sample pretreatment and storage is also briefly discussed.

OBJECTIVE:To develop a method for the simultaneous determination of 67 pesticides in water by solid phase extration(SPE) disk extraction-gas chromatography-tandem mass spectrometry(GC-MS/MS).METHODS:Pesticides in water were extracted and cleaned-up with SPE disk, then eluted with dichloromethane-n-ethyl acetate(7∶3, V/V). After the eluent being concentrated to 1 mL under nitrogen blow at 40 ℃, the supernatant was injected into GC-MS/MS for analysis. The GC separation was performed on a DB-5 MS capillary column(30 m×0. 25 mm×0. 25 μm). The pesticides were detected by MS/MS in multiple reaction monitoring(MRM) mode and quantified by working curve method.RESULTS:The linear range of the method for most of the pesticides were in the range of 0. 05-5 μg/L with correlation coefficients of 0. 9924-0. 9999. The quantitative limits(S/N=10) of the method were in the range of 1. 0×10~(-5)-0. 059 μg/L. The recoveries for pesticides were 81. 0%-125. 0% with relative standard deviations of 1. 5%-21. 4%(n=6).CONCLUSION:The method is sensitive, simple, environmentally friendly and suitable to the determination of pesticides in drinking water for rapid screening and quantitative analysis.

OBJECTIVE:To develop a simple and sensitive high performance liquid chromatographic method for simultaneous determination of catechin hydrate, epicatechin, epigallocatechin, epicatechin gallate, epigallocatechin gallate, dihydromyricetin, glycyrrhizic acid and glycyrrhetinic acid in healthy food for anti-hangover and hepatoprotection, and compare with the capillary electrophoresis method established by our laboratory.METHODS:The samples were ultrasonically extracted by using methanol-water( 4∶ 1, V/V) for 30 minutes and then centrifuged at 10 000 r/min for 10 minutes. The supernatant was filtered and injected into the HPLC system and then separated on a C_(18) column( 5 μm × 250 mm × 4. 6 mm) at 30℃ with gradient elution at a flow rate of 0. 8mL/min. Catechins and dihydromyricetin were detected at the wavelength of 210 nm, glycyrrhizic acid and glycyrrhetinic acid were detected at 250 nm.RESULTS:Under the optimal analytical conditions, the peak area of each analyte and its concentration had agood correlation within the linear range( r ≥ 0. 9996). The limits of detection and quantification of the method were 0. 07-1. 25 μg/g( S/N = 3) and 0. 22-4. 18 μg/g( S/N = 10), respectively. The intra-and inter-day relative standard deviations( RSDs)of the mixed standard solution were 0. 26%-1. 95% and 1. 17%-3. 89%, respectively. The spiked recoveries of the analytes were 86. 15%-98. 61%.CONCLUSION:The established method is sensitive and reliable, and could be used for quality control of the healthy food for anti-hangover and hepatoprotection.

Objective To establish the high-performance chromatographic method for simultaneous determination of ten plant regulators including thidiazuron,forchlorfenuron,abscisic acid,6-glycosyl amino purine,N6-Isoprene adenine,6-Benzyl amino purine,indole-3-butyric acid,indole-3-acetic acid,α-naphthaleneacetic acid,methyl 1-naphthylacetate in vegetables.Methods The plant regulators residues in samples were extracted by acetonitrile,and the excess acetonitrile was removed by evaporation.The residues were then dissolved in dichloromethane.The solution was cleaned up with NH2 cartridge.The analytes were eluted by methanol,and then concentrated.Chromatographic analysis was carried out on Agilent C18 column by methanol/water(0.1％ HCOOH) in gradient program,using both DAD and FLD as detectors.The retention time was qualitative,and the standard curve external standard method was used to quantify the retention time.Results The detection limits of 10 regulators were within 1.0 μg/kg-8.0 μg/kg.When the concentrations were within 0.020 μg/ml-5.00 μg/ml,the correlation coefficient(r) was above 0.999.The recoveries were within 70％-104％,the RSD of precision was less than 4.0％.Conclusion The method is simple with good sensitivity and reproducibility.The practical application brings less detection cost and period.It is suitable for primary units to popularize.

OBJECTIVES:To develop a rapid method of high performance liquid chromatography coupled with variable wave length UV detection for simultaneous determination of 9 natural functional ingredients including puerarin, silymarin, quercetin hydrate, schisandrol A, curcumin, tanshinoneI, tanshinoneIIA, cryptotanshinone, and dihydrotanshinoneIin functional food for anti-hangover and hepatoprotection.METHODS:The samples were ultrasonically extracted with 90 % ethanol (V/V) and centrifuged at 10 000 r/min for 10 min prior to HPLC analysis. The nine target analytes were separated on a C18 column with gradient elution using methanol and water (The pH value was adjusted to 2.5 using H3PO4) as the mobile phase. Qualitative analysis was carried out using retention times of the chromatographic peaks, while the external standard curves were established for quantification.RESULTS:Under the optimal analytical conditions, the peak area of each analyte and its concentration had a good correlation within the linear range ( r≥0.998). The limits of detection and quantification of the method were 0.38-0.73 mg/kg (S/N=3) and 1.27-2.43 mg/kg (S/N=10), respectively. The spiked recoveries of the analytes were 88.9%-103.2%, and the relative standard deviations were 1.3%-3.7%.CONCLUSIONS:The method for the determination of 9 functional ingredients in functional food for anti-hangover and hepatoprotection was proposed for the first time in this study. The results showed that it could meet the requirement of routine analysis and quality control and evaluation.

A rapid method of micellar electrokinetic capillary electrophoresis (CE) coupled with diode array detection was developed for simultaneous determination of catechin, epicatechin, epigallocatechin, epicatechin gallate, epigallocatechin gallate, dihydromyricetin and glycyrrhizic acid in functional food for anti-hangover and hepatoprotection. The parameters of capillary electrophoresis, including buffer concentration, concentration of sodium dodecyl sulfate (SDS), volume ratio of acetonitrile, and pH of the buffer, were optimized with orthogonal design. Under the optimal analytical conditions, the peak area of each analyte and its concentration had a good correlation within the linear range (r >= 0.9989). Limit of detection (LOD) and quantification (LOQ) of the method were in the range of 0.26-2.22 mu g/g (S/N = 3) and 0.87-7.39 mu g/g (S/N = 10), respectively. The intra- and inter-day relative standard deviations (RSDs) of the mixed standard solution were 1.3%-2.5% and 1.9%-3.9%, respectively. While the spiked recoveries of the analytes were 91.4%-104.9% and the RSDs of the spiked samples were 1.4%-3.2%. The method of capillary electrophoresis for determination of the 7 components in functional food for anti. hangover and hepatoprotection was proposed in this study and could achieve baseline separation for all the target components within 8 min. The results show that the method could meet the requirement for routine analysis and quality control and evaluation.