气相色谱法测定胶粘剂中的游离甲醛

采用超声波萃取胶粘剂中游离甲醛,经2,4-二硝基苯肼衍生后用气相色谱一电子捕获检测器法测定．对提取方法、衍生化条件及色谱条件进行了研究,确定了甲醛检测的最佳条件．研究数据显示,该方法对甲醛的检出限为0．175μLg／g,在0．1～60．0μg／mL浓度范围内,线性相关系数R^2=0．9999;在1、2和8μg／mL3个添加水平下的添加回收率在98．97％-102．24％之间,5个实验室对同一样品中甲醛含量测定值的相对标准偏差为4．0％．结果表明本方法简便、快速、检测限低、回收率高、重现性好．     

高效液相色谱法测定禽蛋及其制品中的三聚氰胺

建立了高效液相色谱测定禽蛋类及加工品中三聚氰胺的检测方法．以经三聚氰胺标准添加的鸡蛋、咸鸭蛋和松花蛋为代表性样品,优化了提取溶剂的种类、用量和提取时间条件,探讨了直接过滤、正己烷反萃和固相萃取三种前处理方式的净化效果,并考察了测定时流动相比例和缓冲液的pH条件．实验结果表明：当添加浓度为0．20和10．0μg／g时,三聚氰胺的回收率分别为87．6％-101．5％,测量标准偏差为1．6％～2．8％,方法检出限为0．05μg／g．标准溶液在0．10～2．00μg／mL范围内,线性关系良好,相关系数r=0．9999．利用本方法对12个实际禽蛋样品进行测定,结果表明能够满足禽蛋及其制品中三聚氰胺残留的快速筛查要求．     

高效液相色谱法测定蜜蜂蜂体王浆酸

建立了蜂体中10－HDA的高效液相色谱分析方法。对10－HDA的提取方法进行了研究。在选择的最佳色谱条件下,线性范围为10～1000ng,r=0．9998,回收率96．5％～99．2％,检测限为0.53μg／g。     

高效液相色谱同时测定鸡蛋中4种氟喹诺酮类药物残留

建立了固相萃取—反相高效液相色谱同时分析鸡蛋样品中4种氟喹诺酮类药物残留量的方法。对鸡蛋样品的提取及其在C18固相萃取柱上的净化条件进行了研究,采用高效液相色谱分离,荧光检测器检测(λex=280nm,λem=450nm),外标法定量。4种沙星标准曲线的线性回归系数均在0．9999以上,环丙沙星、恩诺沙星、沙拉沙星的线性范围为2．5～500μg／L;达诺沙星为0．5～100μg/L。鸡蛋样品中4种沙星的加标回收率为78．1％～95．7％;相对标准偏差为4．1％～16．2％。环丙沙星、恩诺沙星、沙拉沙星的最低检出限为10μg／kg;达诺沙星的最低检出限为2μg/kg。     

HPLC法测定食用香菇中的甲醛

建立了用高效液相色谱测定食用香菇中甲醛的方法。将食用香菇用水提取,提取液经2,4-二硝基苯肼(DNPH)衍生后,用高效液相色谱法测定其中的甲醛。外标法定量测定时,甲醛标准溶液的峰面积与样品质量浓度在10．7～856μg／L范围内呈良好的线性关系,线性回归系数(r2)为0．9998,方法的检出限为8．2μg／L。所测定的6种香菇样品中甲醛的平均加标回收率为72％～93％;相对标准偏差为1％～8％。除了一种野生香菇样品未检出外,其它5种市售香菇样品中甲醛的质量分数为34～292mg／kg。     

多功能柱净化-高效液相色谱法检测谷物中的玉米赤霉烯酮

建立了玉米和小麦中玉米赤霉烯酮（ZEN）的多功能柱净化-高效液相色谱检测方法。样品经乙腈-水混合溶剂（V（乙腈）：V（水）=84：16）提取，通过多功能净化柱（MFC）进行一次性净化，以Symmetry^R C18柱为分离柱，甲醇-水（V（甲醇）：V（水）=68：32）为流动相进行高效液相色谱分离和检测。玉米赤霉烯酮的质量浓度在0．01～4．0μg／mL范围内呈良好线性，相关系数为0．9996。检出限为0．04μg／g，在0、04—5．0mg／kg添加范围内的回收率为87．5％～98．6％，相对标准偏差为1．5％～8．3％。     

多功能柱净化-高效液相色谱法同时检测小麦中雪腐镰刀菌烯醇和脱氧雪腐镰刀菌烯醇

建立了小麦中雪腐镰刀菌烯醇（NIV）和脱氧雪腐镰刀菌烯醇（DON）的高效液相色谱同时检测方法。样品采用乙腈-水（体积比85：15）混合溶剂进行提取．通过多功能净化柱（MFC）进行一次性净化，以C18柱为分离柱，水-乙腈-甲醇（体积比90：5：5）混合溶剂为流动相进行高效液相色谱分离和检测。在小麦样品中，本方法在0．2～5μg／g添加范围内的凹收率为87％～99％；相对标准偏差为1．5％～8．3％；DON和NIV的检出限分别为0．12和0、16μg／g（5／N=3）。     

谷物中脱氧雪腐镰刀菌烯醇的高效液相色谱检测及质谱确证

建立了谷物中脱氧雪腐镰刀菌烯醇DON的高效液相色谱检测和质谱确证方法。样品用水提取,通过免疫亲和柱进行富集和净化,以Hypersil BDS C18柱为分离柱,乙腈-水（10：90,V/V）混合溶剂为流动相进行高效液相色谱分离和检测,利用大气压化学电离质谱（APCI）进行阻性结果的鉴定和确认。在小麦、大麦和面粉等样品中,本方法在0．1～10μg／g添加范围内的回收率为82．4％-103％,相对标准偏差1．4％-7．6％,检出限0．1μg／g。     

高效液相色谱法测定食品中的甜蜜素

利用次氯酸钠将食品中的甜蜜素转化为N,N-二氯环己胺,以正己烷萃取后用高效液相色谱法测定。采用Extend-C18 5μm不锈钢柱,以甲醇-水(体积比为80：20)作流动相,二极管阵列检测器检测波长为314nm。甜蜜素的浓度在1～80μg／mL内与色谱峰面积成良好的线性关系,回收率为102．8％～103．0％,检出限为1μg／mL,测定结果的相对标准偏差为0．84％。     

反胶束萃取-高效液相色谱法测定磺酸型偶氮染料

建立了水中磺酸偶氮染料甲基橙（MO）、刚果红（CR）和酸性铬兰K（ACBK）的反胶束萃取-离子对高效液相色谱定量检测的方法。采用Hypersil C18柱（250×4．6mm,5μm）,流动相为V（甲醇）／V（水）=63：37（含10mmol／L的KH2PO4、4mmol／L的四丁基溴化铵,KOH调pH=7．0）,流速为0.8mL／min,MO、CR和ACBK检测波长分别为449nm、505nm和526nm。结果表明,染料的回收率为92．9％～102．1％,相对标准偏差为0．9％～2．3％,水中MO、CR和ACBK的检出限分别为0．6μg／L、1．2μg／L和1．3μg／L。     

气相色谱法同时测定溶剂型胶黏剂中的9种有害物质

建立了利用毛细管柱气相色谱同时测定溶剂型胶黏剂中苯、 甲苯、 对（间）二甲苯、 邻二甲苯、 二氯甲烷、1,2-二氯乙烷、1,1,2-三氯乙烷、三氯乙烯、甲苯二异氰酸酯（TDI）的方法,并对样品中有害物质的分离提取和色谱条件进行了研究.实验结果表明,方法化合物浓度在10~300 μg/mL时,线性相关系数不低于0.999 1,样品加标回收率在91.2%~104.1%之间,相对标准偏差均小于5%,检出限为0.1~3.0 μg/mL.方法不仅回收率高、重现性好,而且简便、快速.     

Simple high‐performance liquid chromatography method for formaldehyde determination in human tissue through derivatization with 2,4‐dinitrophenylhydrazine

A simple high‐performance liquid chromatography method has been developed for the determination of formaldehyde in human tissue. FA Formaldehyde was derivatized with 2,4‐dinitrophenylhydrazine. It was extracted from human tissue with ethyl acetate by liquid–liquid extraction and analyzed by high‐performance liquid chromatography. The calibration curve was linear in the concentration range of 5.0–200 μg/mL. Intra‐ and interday precision values for formaldehyde in tissue were <6.9%, and accuracy (relative error) was better than 6.5%. The extraction recoveries of formaldehyde from human tissue were between 88 and 98%. The limits of detection and quantification of formaldehyde were 1.5 and 5.0 μg/mL, respectively. Also, this assay was applied to liver samples taken from a biopsy material.     

柱前衍生-萃取阻断反应-高效液相色谱法测定化妆品中游离甲醛

建立了柱前衍生化-萃取阻断反应-高效液相色谱(HPLC)测定化妆品中甲醛的方法。化妆品中甲醛检测的难点是: 甲醛缓释剂类防腐剂在衍生过程中释放甲醛,影响游离甲醛的准确测定。以2,4-二硝基苯肼(DNPH)乙腈溶液-磷酸盐缓冲液(pH 2)(1:1, v/v)为提取溶液,于室温下快速衍生2 min后,立即加入二氯甲烷萃取,阻断衍生反应,经乙腈稀释后进行HPLC测定。以Agilent C18柱(250 mm×4.6 mm, 5 μm)为分离柱,乙腈-水(60:40, v/v)为流动相,流速为1.0 mL/min,于355 nm波长下检测。在洗发水、乳液、膏霜、洗手液、牙膏、指甲油、粉饼中分别添加50、100、500、1000 μg/g 4个浓度水平的甲醛,其回收率为81%～106%,相对标准偏差(n=6)＜5.0%。方法的定量限(以信噪比(S/N)＞10计)为50 μg/g。该方法快速、简便、重现性好,且可以有效避免甲醛缓释剂类防腐剂分解释放甲醛,适用于化妆品中游离甲醛的测定。     

Simultaneous determination of tetrahydropalmatine and tetrahydroberberine in rat urine using dispersive liquid-liquid microextraction coupled with high-performance liquid chromatography

Dispersive liquid-liquid microextraction (DLLME) coupled with high-performance liquid chromatography (HPLC)-UV detection was applied in rat urine for the extraction and determination of tetrahydropalmatine (THP) and tetrahydroberberine (THB), both active components in Rhizoma corydalis. Various parameters affecting the extraction efficiency, such as the type and volume of extraction and dispersive solvent, pH, etc. were evaluated. Under the optimal conditions (extraction solvent: 37 μL of chloroform, dispersive solvent: 100 μL of methanol, alkaline with 100 μL of 1 mol/L NaOH, and without salt addition), the enrichment factors of THP and THB were more than 30. The extraction recoveries were 69.8-75.8% and 72.7-77.6% for THP and THB in rat urine, respectively. Both THP and THB showed good linearity in the range of 0.025-2.5 μg/mL, and the limit of quantification was 0.025 μg/mL (S/N=10, n=6). The intra-day and inter-day precision of THP and THB were <12.6%. The relative recoveries ranged from 95.5 to 107.4% and 96.8 to 100.9% for THP and THB in rat urine, respectively. The method has been successfully applied to rat urine samples. The results demonstrated that DLLME is a very simple, rapid and efficient method for the extraction and preconcentration of THP and THB from urine samples.     

Extraction and preconcentration of formaldehyde in water by polypyrrole‐coated magnetic nanoparticles and determination by high‐performance liquid chromatography

In this study, a simple and rapid extraction method based on the application of polypyrrole‐coated Fe₃O₄ nanoparticles as a magnetic solid‐phase extraction sorbent was successfully developed for the extraction and preconcentration of trace amounts of formaldehyde after derivatization with 2,4‐dinitrophenylhydrazine. The analyses were performed by high‐performance liquid chromatography followed by UV detection. Several variables affecting the extraction efficiency of the formaldehyde, i.e., sample pH, amount of sorbent, salt concentration, extraction time and desorption conditions were investigated and optimized. The best working conditions were as follows: sample pH, 5; amount of sorbent, 40 mg; NaCl concentration, 20% w/v; sample volume, 20 mL; extraction time, 12 min; and 100 μL of methanol for desorption of the formaldehyde within 3 min. Under the optimal conditions, the performance of the proposed method was studied in terms of linear dynamic range (10–500 μg/L), correlation coefficient (R² ≥ 0.998), precision (RSD% ≤ 5.5) and limit of detection (4 μg/L). Finally, the developed method was successfully applied for extraction and determination of formaldehyde in tap, rain and tomato water samples, and satisfactory results were obtained.     

超声萃取-高效液相色谱法测定烟草中β-D-吡喃葡萄糖-3-氧代-α-紫罗兰醇苷

建立了一种用超声波辅助萃取-高效液相法测定烟草中β-D-吡喃葡萄糖-3-氧代-α-紫罗兰醇苷含量的新方法。以甲醇为萃取溶剂,超声萃取条件经过正交实验优化,优化后的条件为料液比1:40(m/V,g/mL)、萃取功率160W,萃取时间20 min。所得萃取液经大孔吸附树脂柱层析法分离后,用Waters SunFireC18(150 mm×4.6 mm,5μm)色谱柱分离,紫外检测器(波长为243nm)检测,流动相为V(乙腈):V(水)=20:80;流速1 mL/min。β-D-吡喃葡萄糖-3-氧代-α-紫罗兰醇苷在0.01～1 mg/mL范围内线性关系良好,相关系数为0.9994,相对标准偏差为1.8%,检出限为0.05μg/mL,平均回收率为87.80%。该方法适用于β-D-吡喃葡萄糖-3-氧代-α-紫罗兰醇苷的定量分析。     

Validation of a high-performance chromatographic method for determination of cefotaxime in biological samples

An analytical method for detecting and quantifying cefotaxime in plasma and several tissues is described. The method was developed and validated using plasma and tissues of rats. The samples were analyzed by reversed phase liquid chromatography (HPLC) with UV detection (254 nm). Calibration graphs showed a linear correlation (r > 0.999) over the concentration ranges of 0.5–200 μg/mL and 1.25–25 μg/g for plasma and tissues, respectively. The recovery of cefotaxime from plasma standards prepared at the concentrations of 25 μg/mL and 100 μg/mL was 98.5 ± 3.5% and 101.8 ± 2.2%, respectively. The recovery of cefotaxime from tissue standards of liver, fat and muscle, prepared at the concentration of 10 μg/g was: 89.8 ± 1.2% (liver), 103.9 ± 6.5% (fat) and 97.8 ± 2.1% (muscle). The detection (LOD) and quantitation (LOQ) limits for plasma samples were established at 0.11 μg/mL and 0.49 μg/mL, respectively. The values of these limits for tissues samples were approximately 2.5 times higher: 0.3 μg/g (LOD) and 1.25 μg/g (LOQ). For plasma samples, the deviation of the observed concentration from the nominal concentration was less than 5% and the coefficient of variation for within-day and between-day assays was less than 6% and 12%, respectively. The method was used in a pharmacokinetic study of cefotaxime in the rat and the mean values of the pharmacokinetic parameters are given.     

浊点萃取-高效液相色谱法检测牛奶中的六种农药

建立了应用浊点萃取法对牛奶中的残留除草剂进行萃取富集后用高效液相色谱(HPLC)检测的方法。以60 g/L的表面活性剂Tween 20或Triton X-100为萃取剂,在一定浓度的(NH4)2SO4或NaCl的存在下加热萃取。牛奶中6种不同的除草剂被胶束相富集后被HPLC分离检测。结果表明:肟草酮、嗪草酮和溴苯腈在20～10000 μg/L、苯噻草胺在30～10000 μg/L、苄嘧磺隆和烟嘧磺隆在50～10000 μg/L时其浓度和检测信号呈线性关系,相关系数为0.9981～0.9997,平均加标回收率为85.09%～96.74%,相对标准偏差为1.90%～3.98%。6种农药的定量检测限均小于国家规定的农药残留限量(MRL)。该方法简便、快速、灵敏、污染少,实际应用性好。     

双水相萃取-高效液相色谱法测定酵母细胞中麦角固醇含量

建立了乙醇-水双水相萃取-高效液相色谱法测定酵母细胞中麦角固醇含量的分析方法。先使酵母细胞在KOH-乙醇溶液中于85℃~90℃回流皂化2 h,冷却后加入适量分相剂Na3PO4.12H2O使其形成双水相体系,经振摇萃取,麦角固醇进入乙醇相,萃取效率为95%~102%。用高效液相色谱法(HPLC)测定醇相中麦角固醇含量,采用DiamonsilTMC18色谱柱(200×4.6 mm,5μm),流动相为甲醇,流速为1.0 mL/min;紫外检测波长为281 nm,进样量为20μL。方法线性范围为30.15~2010μg/mL,检出限为1.3μg/mL;用其测得酵母细胞中麦角固醇含量为2.74 mg/g,RSD为2.1%(n=5),加标回收率为91.6%~96.9%。