Uncertainty Evaluation of Determination of Microcystin MC-LR in Environmental Samples by Solid Phase Extraction-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

To assess uncertainty of determination of MC-LR in environmental samples by solid phase extraction- ultra performance liquid chromatography- tandem mass spectrometry,the sources of the uncertainty were evaluated firstly,and the expanded uncertainty was calculated finally.The results show that when MC-LR concentration in the water samples was 0.50 μg/L,the expanded uncertainty was 0.00628 μg/L(k=2).

Rapid Quantitative Determination of Isoprene Monomer in Living Taraxacum kok-saghyz by Ultra-High Performance Liquid Chromatography Tandem Mass Spectrometry

Taraxacum kok-saghyz(TKS)is rich in natural rubber(NR),a natural organic macromolecular compound composed of cis-1,4-polyisoprene,and may become the second NR-bearing plant for biochemical engineering development.In this paper,a rapid and quantitative ultra-high performance liquid chromatography tandem mass spectrometry(UHPLCMS/MS)method was established for determination of macromolecular biosynthesis substrate(dimethylallyl pyrophosphate,DMAPP)and initiator(farnesyl pyrophosphate,FPP)contained in TKS.A Kromasil C18 chromatographic column was used for separation,and the multi-reaction monitoring mode(MRM)of triple quadrupole mass spectrometry was used for detection.Quantification was performed by external calibration method.The results showed that the limit of detection(LOD)and the limit of quantitation(LOQ)of DMAPP were 2.42μg/L and 7.26μg/L,respectively,and the LOQ and the LOD of FPP were 1.02μg/L and 3.05μg/L,respectively.At a concentration of 1—1000μg/L,both analytes had good determination coefficients(>0.999)of calibration curve.The recoveries of DMAPP and FPP were between 99.0%and 117.1%.In real samples detection,the contents of DMAPP and FPP in TKS samples were between 23.32—82.77μg/L and 12.03—85.67μg/L,respectively.Thus,this approach is a reliable method to quantify DMAPP and FPP in TKS.

Modernization of Chinese herbal compound and the high performance liquid chromatography tandem mass spectrometry (HPLC-MS)

Chinese herbal compound is playing an important role on curing human diseases.And it has been a trend that Chinese herbal compound is being used all over the world in 21 century.However,our Chinese herbal compound is facing serious challenge for the lack of canonical system of quality criterion for Chinese herbal compound so it has been a urgent problem to set up the quality control standards and reveal therapeutic basis of Chinese herbal compound.In order to give full play to the advantages of Chinese herbal compound,modern scientific and technological is used to research of Chinese herbal compound,especially the high performance liquid chromatography tandem mass spectrometry(HPLC-MS),because it is high sensitive,rapid,and obtain more information.It is very necessary that HPLC-MS is uesed to elucidate the effective components of basic substances of Chinese Herbal Compound,and endow traditional Chinese medicine with modern scientific connotation.

Determination of thyreostats in bovine urine using ultra-high performance liquid chromatography-tandem mass spectrometry

Five thyreostats(TSs),namely tapazole,thiouracil,methylthiouracil,propylthiouracil,and phenylthiouracil,were determined in bovine urine using ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS)in positive electrospray ionization mode.Extraction and clean-up were achieved using a ChemElut cartridge with tert-butyl methyl ether,without a derivatization step.Separation was achieved on an Acquity UPLC SS T3 column.The mobile phase was acetonitrile and water containing 0.2%(v/v)formic acid.The mass spectrometer was operated in multiple reaction monitoring mode.Urine samples were spiked with TS solution at levels corresponding to 5,10,15,and 20μg/L.The accuracy(internal standard corrected)ranged from 92%to 107%,with a repeatability precision(relative standard deviation,RSD)less than 15%for all five analytes.The RSDs within-laboratory reproducibility was less than 26%.The decision limits(CCα)and detection capabilities(CCβ)were obtained from a calibration curve and were in the ranges of 3.1-6.1μg/L and 4.0-7.4μg/L,respectively.The CCαand CCβvalues were below the recommended concentration,which was set at 10μg/L.The results show that the described method is suitable for the direct detection of TSs in bovine urine.This method can also be used to determine TSs in porcine urine.

Determination of Oleuropein in Cosmetics by Ultra Performance Liquid Chromatography-Triple Quadrupole Tandem Mass Spectrometry

An ultrahigh performance liquid chromatography-triple quadrupole tandem mass spectrometry(UPLC-MS/MS)was established to quickly and accurately determine the content of oleuropein in cosmetics.The samples were extracted with methanol-aqueous solution,and the mobile phase with methanol-formic acid solution(0.1 mol/L)=40∶60 was separated by Agilent ZORBAX Eclipse Plus C18(2.1 mm×50 mm×1.8μm-Micron)column temperature 30℃,flow rate 0.3 mL/min.The MS end was detected by electrospray negative mode ionization(ESI-)and multiple reaction monitoring(MRM)mode.The results show a good linear relationship in the range of 0.002~5 mg/L,with a correlation coefficient R2 of 0.999,5.Method recovery range from 84.2%~107.6%and the relative standard deviation RSD is 5.8%.The detection time is 5 min,the detection limit is 0.000,6 mg/L,and the limit of quantification is 0.002 mg/L.This method has the advantages of convenient operation,low quantification limit,high precision and good repeatability,and is suitable for measuring the content of oleuropein in many kinds of cosmetics.

Determination of okadaic acid related toxins from shellfish (<i>sinonovacula constricta</i>) by high performance liquid chromatography tandem mass spectrometry

Consumption of shellfish contaminated with algal toxins produced by marine dinoflagellates can lead to diarrhetic shellfish poisoning (DSP). It was therefore essential that there are analytical techniques to identify and quantify DSP toxins in shellfish. This new methodology could facilitate DSP monitoring and create a means of rapidly responding to incidents threatening public health. In the last years there were different analytical methods for DSP, such as mouse bioassay and LC-FLD. With the development of instrument, Liquid chromatography-mass spectrometry was substituted for other analytical methods with its good sensitivity and selectivity and without derivatization for the determination of DSP. In this report, a high performance liquid chromatogra-phytandem mass spectrometric(HPLC-MS/MS)method was developed for the simultaneous determination of okadaic acid (OA) and dinophysistoxins(DTX1) in Sinonovacula constricta. Optimization of pretreatment experiment was carried out to maximize recoveries and the effectiveness. The analytes were determined under multi-reactions monitoring (MRM) scan type with tandem mass analyzer using negative ion electrospray ionization (-ESI) mode .Finally, the detection and identification of OA and DTX-1 were based upon their retention times (RT) and the fragmentation patterns of their mass spectra. The method of LOQ for the two poisons was 0.02 mg·kg-1.The real sample test showed that this method could be used for sensitive, fast, and accurate determination of the two diarrheic shellfish poisons in shellfish.

Determination of 24 Allergens in Perfume with High Performance Liquid Chromatography Tandem Mass Spectrometry

A method of 24 allergens determination in cosmetics were established with high performance liquid chromatography tandem mass spectrometry. The targeted compounds were extracted with acetonitrile and determined with LC-MS/MS (MRM mode) with external method. The linearity between concentrations and peak area ratio was obtained from 1.0~5.0 mg/L. The limits of detection were 1.0 mg/L for the instrument and 5.0 mg/kg for the method respectively. The LOQ was 15.0 mg/L. The average recoveries of 24 allergens were between 85.9% and 110.0% at spiked levels of 5, 10 and 20 mg/kg with relative standard derivation (RSDs) of 5.5%~12.0%(n=10). The method could be used as a reliable means for simultaneous quantitative determination of allergens in cosmetics.

Rapid Determination of Three Kinds of Microcystins in Environmental Water Samples by Disk SPE-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

A method of rapidly detecting three kinds of microcystins( MCs) in environmental water samples by using disk SPE- ultra high performance liquid chromatography- tandem mass spectrometry( UPLC- MS / MS) was established. Firstly,environmental water samples were extracted by disk SPE column( C_(18)),and three kinds of MCs were separated by Waters BEH C_(18) chromatographic column with acetonitrile- 0. 2% formic acid solution as the mobile phase. After the gradient elution separation,the external standard method was used for quantitative and qualitative analysis under MRM of UPLC- MS / MS. The results showed that the three kinds of MCs in the range of 0. 05- 10 μg / L showed good linear relation,and the correlation coefficients were higher than 0. 999 4,while the method detection limit was 0. 04 ng / L. Under 0. 1,1,and 5 μg / L standard addition for the same environmental sample,the average recovery was 82. 8%- 108. 8%,and the relative standard deviation of determination results was2. 1%- 10. 1%( n = 6). This method is rapid,sensitive and accurate,so it can be effectively applied in the monitoring of MCs in environmental water samples.

液液萃取-超高效液相色谱-串联质谱法同时测定尿液中乌头碱和新乌头碱

建立液液萃取-超高效液相色谱-串联质谱法同时测定尿液中乌头碱和新乌头碱的含量。向尿液样品中加入一定量的萃取溶剂,涡旋,离心,取上层有机相,重复萃取两次,合并萃取液,氮吹至干,再复溶于乙腈中。以乙腈和含0.1%甲酸的2 mmol/L甲酸铵溶液作为流动相,梯度洗脱,采用Acquity BEH C_(18)色谱柱分离,电喷雾离子源正离子方式扫描,多反应监测模式监测,以保留时间和特征离子定性,外标法定量。乌头碱和新乌头碱的质量浓度在1.0~100.0μg/L范围内与其色谱峰面积呈良好的线性关系,相关系数均不小于0.998,方法检出限为0.01μg/L。样品加标平均回收率为99.2%~105.4%,测定结果的相对标准偏差为1.7%~4.1%(n=5)。该方法灵敏度高,准确可靠,适用于食物中毒患者尿液中乌头碱和新乌头碱的检测。

超高效液相色谱-串联质谱测定胆石症患者血清胆汁酸谱的意义及价值

目的:探究超高效液相色谱-串联质谱测定胆石症患者血清胆汁酸谱的意义及价值。方法:选取2023年7月至12月收治的83例胆石症患者资料进行回顾性分析,并按1∶1比例选取同期体检健康者83例为对照组。比较两组受试者血清初级胆汁酸谱、次级胆汁酸谱差异,分析胆石症影响因素及胆汁酸谱诊断胆石症的价值效能。结果:研究组受试者牛磺胆酸(TCA)、甘氨鹅脱氧胆酸(GCDCA)、甘氨胆酸(GCA)、甘氨熊脱氧胆酸(GUDCA)、牛磺熊去氧胆酸(TUDCA)、牛磺鹅去氧胆酸(TCDCA)高于对照组,差异有统计学意义(P<0.05)。二元Logistic回归分析显示,TCA、GCDCA、GCA、TUDCA、TCDCA均是胆石症发生的危险因素(P<0.05)。ROC曲线分析显示,TCA、GCDCA、GCA、TUDCA、TCDCA诊断胆石症的AUC分别为0.760、0.755、0.914、0.855、0.880,联合数据诊断胆石症的的AUC分别为0.921,敏感度为91.6%,特异度为97.6%。结论:胆石症患者血清胆汁酸谱存在异常,超高效液相色谱-串联质谱测定的血清胆汁酸谱可作为评估胆石症的有效方式之一,为临床早期预防提供参考。

固相萃取-超高效液相色谱-串联质谱法测定猪肉中9种氨基糖苷类抗生素残留

建立了猪肉样品中痕量氨基糖苷类抗生素(Aminoglycosides,AGs)(阿米卡星、安普霉素、潮霉素B、卡那霉素、巴龙霉素、核糖霉素、大观霉素、链霉素、妥布霉素)残留的检测方法。猪肉样品经过冷冻干燥、研磨后,加入150 mmol/L EDTA溶液和5%TCA溶液进行超声提取,经Oasis HLB柱净化后,采用BEH Z-HILIC色谱柱,进行超高效液相色谱-串联质谱分析。9种AGs在0.01~5μg/mL范围内线性关系良好,相关系数(R^(2))均大于0.999。猪肉样品中AGs的定量限为0.01~0.29μg/g。在低、中、高3种加标水平下,猪肉样品中AGs的平均加标回收率为79.91%~113.20%,相对标准偏差为1.26%~12.40%。该方法操作简单、灵敏度高,适用于猪肉中AGs残留的检测。

基于肠道菌群和广泛靶向代谢组学的山柰酚抗骨质疏松的作用机制

背景:山柰酚具有抗骨质疏松的作用,但山柰酚通过调控肠道菌群、代谢物防治骨质疏松的作用机制尚不明确。目的:基于肠道菌群和广泛靶向代谢组学探究山柰酚抗骨质疏松的可能作用机制。方法:将雌性Sprague-Dawley大鼠18只随机分为假手术组、模型组和山柰酚组,每组6只,后2组切除双侧卵巢制备骨质疏松大鼠模型。造模后8周,假手术组和模型组采用蒸馏水灌胃,山柰酚组采用40 mg/kg山柰酚灌胃,各组均连续给药12周。取大鼠粪便进行16SrDNA扩增子测序,观察肠道菌群结构的变化;采用超高效液相色谱-串联质谱技术、自主开发的数据库和多元统计分析的方法进行血清样本广泛靶向代谢组学检测。结果与结论:①连续干预12周后,16SrDNA扩增子测序结果显示,与假手术组相比,模型组肠道菌群丰度增加;与模型组相比,山柰酚组上调Latilactobacillus菌属(P=0.021)丰度,下调泛菌属(Pantoea)(P=0.034)、肠杆菌属(Enterorhabdus)(P=0.000)、Monoglobus菌属(P=0.024)、丁酸单胞菌属(Butyricimonas)(P=0.034)、Rothi属(P=0.043)、梭杆菌属(Clostridia)(P=0.004)等菌属丰度。②连续干预12周后,血清样本广泛靶向代谢组学检测结果显示,假手术组与模型组、模型组与山柰酚组之间分别鉴定出120和79种代谢物,3组间共有17种交集差异代谢物,包括乌头酸、巴比妥酸、L-高瓜氨酸、3,4,5-三甲氧基肉桂酸、L-3-苯基乳酸、环(脯氨酸-脯氨酸)、L-苯丙氨酸-L-丝氨酸、脯氨酸-异亮氨酸、L-冬胺基乙酸-L-苯丙胺基乙酸、苯丙氨酸-天冬氨酸等。大部分属于氨基酸及其代谢物、甘油磷脂类和脂肪酰类。差异代谢物涉及的KEGG通路主要富集在D-氨基酸代谢、组氨酸代谢、丙酸代谢、赖氨酸降解、脂肪酸代谢、鞘脂代谢等。③连续干预12周后,联合分析发现,肠杆菌属(Enterorhabdus)、Latilactobacillus属、Rothia属和瘤胃球菌属(Ruminococcus)等与血清差异代谢物密切相关。④山柰酚可能通过调节肠道菌群的丰度、多样性及结构,调控氨基酸及其代谢物的代谢、脂肪酸代谢等发挥抗骨质疏松的作用。

高效液相色谱-串联质谱法测定鸡蛋中18种拟除虫菊酯类农药残留

基于高效液相色谱-串联质谱法(LC-MS/MS)建立同时测定鸡蛋中18种拟除虫菊酯类农药残留的方法。样品经10 mL乙腈提取,弗罗里硅土固相萃取柱净化,以5 mmol/L乙酸铵溶液(A)-甲醇(B)作为流动相进行梯度洗脱,在离子源温度450℃时,采用多反应监测模式(MRM)进行定性定量分析。结果表明:18种拟除虫菊酯类农药在质量浓度5.00~200.00μg/L范围内,线性关系良好(r>0.995),检出限为5.00μg/kg,在20.0~100μg/kg加标水平下,回收率为79.2%~107%,相对标准偏差为0.707%~8.91%(n=3)。

高效液相色谱-串联质谱法分析游离RNA修饰核苷的研究进展

核糖核苷酸(RNA)的转录后修饰在基因表达调控中发挥重要作用,而RNA在降解与再合成过程中产生大量游离核苷,包含未修饰的基础核苷和多种类型的修饰核苷。修饰核苷无法被进一步分解,在胞内积累,或在转运蛋白作用下运输到胞外环境,直到被机体代谢,并在过程中发挥信号分子的作用。对生物样本中各级代谢物中修饰核苷的准确鉴定与定量能够为RNA降解和游离修饰核苷排泄调控提供重要信息,协助研究其生物学功能和发现潜在的临床应用。例如,小分子修饰核苷在应激反应和疾病状态下作为信号分子调控机体的应答;病理状态下体液和组织中发生特异性变化的修饰核苷可作为生物标志物,为疾病的诊断和治疗提供信息。高效液相色谱-串联质谱(HPLC-MS/MS)技术作为一种高灵敏度、高选择性、快速高效的分析工具,已在游离修饰核苷分析中展现出重要的应用价值。但HPLC-MS/MS准确分析游离修饰核苷仍面临一些挑战,如生物样品成分的复杂性,多种类目标物的化学性质差异,多种目标物的含量呈数量级的差异,以及众多的修饰核苷中同分异构体的干扰等。这些因素使得开发同时定量多种核苷的HPLC-MS/MS方法难度增加。本综述介绍了内源性游离RNA修饰核苷的来源及检测方法,概述了HPLC-MS/MS技术在内源性核苷分析中的样品前处理、色谱分离、质谱检测模式和定量方法开发等方面的研究进展,并综述了游离RNA修饰核苷的生物学功能、调控机制研究和作为疾病潜在分子标志物等的应用。

弱阳离子交换固相萃取-超高效液相色谱-串联质谱法测定牛奶中13种氨基糖苷类药物残留

本研究建立弱阳离子交换固相萃取-超高效液相色谱-串联质谱测定牛奶中13种氨基糖苷类药物(安普霉素、阿米卡星、巴龙霉素、潮霉素B、核糖霉素、卡那霉素、链霉素、庆大霉素C1、双氢链霉素、妥布霉素、壮观霉素、新霉素和小诺霉素)的检测方法。牛奶样品经乙酸铵缓冲溶液和乙腈提取,弱阳离子交换固相萃取柱净化,SILICA SG80液相色谱柱分离。采用0.1%甲酸溶液和乙腈作为流动相进行梯度洗脱,在电喷雾电离源、正离子模式下进行超高效液相色谱-串联质谱检测,采用基质匹配标准外标法定量。在5.0~500.0 ng/mL范围内,13种氨基糖苷类药物呈现良好的线性关系(R^(2)≥0.998 3)。潮霉素B、核糖霉素、链霉素、妥布霉素和双氢链霉素的检出限均为3μg/kg,定量限均为10μg/kg;安普霉素、阿米卡星、巴龙霉素、卡那霉素、庆大霉素C_(1)、小诺霉素、新霉素和壮观霉素的检出限均为15μg/kg,定量限均为50μg/kg。在1、2倍和5倍的定量限加标水平下,回收率为73.8%~107.4%,相对标准偏差为1.0%~9.8%。该方法灵敏度高、操作简单、稳定性好,可用于检测牛奶中13种氨基糖苷类药物。

超高效液相色谱−串联质谱法测定织纹螺中河豚毒素的方法优化

【背景】近年来,因食用织纹螺引发的河豚毒素(TTX)中毒事件频发,然而现行国家标准(GB 5009.206-2016)中的液相色谱−串联质谱法(LC-MS/MS)仅适用于河鲀中TTX含量的检测,因此亟需建立一种适用于检测织纹螺中TTX含量的高效、准确的方法。【目的】基于超高效液相色谱−串联质谱法(UPLC-MS/MS)建立一种高效且能准确测定织纹螺中TTX含量的方法。【方法】通过比较不同前处理方法(提取溶液、提取方式、冷冻时间)下TTX回收率的大小,以及不同色谱条件(流动相、进样量)对色谱峰的影响,获得最佳实验条件。此外,采用优化后的方法和现行国家标准方法对采自福建省莆田市和宁德市的织纹螺样品进行测定,以比较该检测方法的准确性和可靠性。【结果】最佳前处理条件:样品首先采用0.1%乙酸溶液60℃超声提取20 min,随后使用80%(体积分数)0.1%乙酸甲醇溶液稀释并在−18℃下冷冻30 min后离心,取上清液过膜后,上机测定;UPLC-MS/MS条件:以含5 mmol·L^(−1)乙酸铵的0.1%甲酸溶液和乙腈为流动相,经Amide-80色谱柱梯度洗脱后,采用电喷雾正离子选择反应监测模式,以基质标准曲线外标法定量。TTX在织纹螺中的基质效应为68.9%,在1~100 ng·mL^(−1)基质标准曲线范围内线性关系良好,线性回归方程相关系数R^(2)>0.99。本方法的检出限和定量限分别为10、25μg·kg^(−1),能同时满足中国和欧洲食品安全委员会对水产品中TTX安全限量值(分别为2200、44μg·kg^(−1))的要求。此外,在3个TTX加标浓度(50、500、4000μg·kg^(−1))下,平均回收率为74.8%~104%,相对标准偏差(RSD)均小于15%(n=6)。分别采用优化后的实验方法和现行国家标准方法对9份织纹螺样品进行检测,2种方法检测的TTX含量范围分别为<0.0250~22.8、0.0120~23.5 mg·kg^(−1),相对偏差为1.51%~14.6%,表明本检测方法准确可靠。【结论】本研究优化建立了一种适用于测定织纹螺中TTX含量的UPLC-MS/MS法,具有前处理简单、快速准确和低成本等特点,为实现织纹螺中TTX含量的快速批量检测奠定良好基础。

同位素内标稀释-UPLC-MS/MS法同时测定生活饮用水中5种消毒副产物和高氯酸盐

利用同位素稀释技术建立一种可同时测定生活饮用水中二氯乙酸、三氯乙酸、氯酸盐、亚氯酸盐和溴酸盐5种消毒副产物以及高氯酸盐的超高效液相色谱串联质谱(ID-UPLC-MS/MS)检测方法。样品过膜后加入同位素内标,采用Torus DEA色谱柱(100 mm×2.1 mm,1.7μm)分离,以0.5%氨水-1 mmol/L乙酸铵和乙腈为流动相洗脱,多反应监测(MRM)负模式(ESI-)测定,内标法定量。6种化合物线性相关系数r均大于0.990,检出限为1.5~2.1μg/L,定量限为5.0~7.0μg/L,应用该方法对399份水样进行测定,检出率为16.04%。该方法采用同位素内标稀释直接进样,分析速度快,灵敏度高,数据准确适用于饮用水国家标准(GB/T 5750.5—2023和GB/T 5750.10—2023)检测限值的要求。

基质分散固相萃取结合超高效液相色谱-串联质谱法快速测定红糖中丙烯酰胺

该研究建立了一种基质分散固相萃取结合超高效液相色谱-串联质谱法快速测定红糖中丙烯酰胺的方法。样品加入13C3-丙烯酰胺同位素内标并用水-乙腈溶解,经盐析作用提取到乙腈中,分离乙腈层后,采用SCX+PSA净化,最后利用超高效液相色谱-串联质谱法测定,内标法定量。结果表明,丙烯酰胺在1.0~200 ng·mL^(-1)范围内线性关系良好(r^(2)=0.9994),方法检出限(LOD)和定量限(LOQ)分别为0.78μg·kg^(-1)和2.62μg·kg^(-1)。对两份红糖样品进行6个浓度水平的加标验证,平均回收率介于95.0~99.2%之间,相对标准偏差(RSD)在1.0~2.2%之间。采集不同产地、品牌和性状的红糖样品19份,结果介于136.3~2011.5μg·kg^(-1)之间,多集中在400μg·kg^(-1)附近,存在一定的安全风险。

超高效液相色谱-串联质谱法测定复杂水质中25种全氟/多氟化合物

建立超高效液相色谱-串联质谱测定复杂水质中25种全氟/多氟化合物(PFASs)含量的分析方法。样品经直接过滤、乙腈提取或固相萃取,用Agilent Eclipse Plus C_(18)色谱柱分离,以含0.01%甲酸的甲醇溶液和水作为流动相,梯度洗脱,在电喷雾负离子模式下,采用多反应监测模式检测,用内标法定量。25种PFASs的质量浓度在0.5~100μg/L范围内与色谱峰面积线性关系良好,相关系数均大于0.999,3种样品处理方法的检出限分别为0.06~0.20、0.002~0.006μg/L和0.1~0.2 ng/L。样品加标平均回收率为69.9%~115%,测定结果的相对标准偏差为2.9%~19.6%(n=6)。该方法简单快捷、重现性好、灵敏度较高,适用于氟化工园区污水、地表水和地下水中25种PFASs的测定。

固相萃取-超高效液相色谱-串联质谱法测定蜂蜜中39种植物源性毒素

为有效评估蜂蜜中可能残留多种植物源性毒素的食品安全风险,建立和验证固相萃取-超高效液相色谱-串联质谱测定蜂蜜中39种植物源性毒素的检测方法。试样经0.1%甲酸水提取,HLB小柱净化,多反应监测模式检测,基质匹配外标法定量。本方法中39种植物源性毒素在各自浓度范围内线性关系良好,平均回收率介于78.7%~112.8%,相对标准偏差介于1.6%~15.2%(n=6)。该方法具有操作简单、检测通量大、灵敏度高等特点,能够满足蜂蜜中该类毒素监测的应用需求。在实际36批次样品的检测过程中,部分样品分别检出了不同含量的吡咯里西啶生物碱和闹羊花毒素III,证明蜂蜜中确具有残留该类植物毒素的风险。