目的:建立液相色谱-串联质谱(LC-MS/MS)方法测定金钗石斛类保健食品及其原料中石斛碱含量.方法:样品通过70％甲醇热回流的方法进行处理后,采用Agilent EclipsePlus C18色谱柱,以0.1％甲酸水溶液(A)-乙腈(B)为流动相进行梯度洗脱,流速0.2 mL/min,进样量5μL.利用电喷雾离子源(ESI),采用正离子模式,多反应监测模式(MRM)进行检测,根据保留时间定性,外标法定量.结果:石斛碱的出峰时间在2.949 min,浓度在1.15～115 ng/mL范围内线性关系良好(r=0.9996),检出限为0.0373 ng/mL.金钗石斛原料和金钗石斛软胶囊的平均加标回收率分别为97.85％和102.64％;精密度相对标准偏差(RSD)分别为1.37％和0.97％.结论:该方法具有分析速度快、灵敏度高、重现性好、准确度高的特点,可为金钗石斛类保健食品及其原料的质量控制提供参考.

目的 建立保健食品中六六六、滴滴涕残留量的毛细管气相色谱分析方法.方法 采用DB-1701毛细管色谱柱(30 m×0.25 mm,0.25 μm),检测器为电子捕获检测器(ECD),比较分析了2种不同前处理方法对六六六、滴滴涕残留量测定的影响.结果 六六六的4种异构体和滴滴涕的4种异构体分离良好,峰面积与浓度在0.02 μg/ml ～ 0.06 μg/ml内呈良好的线性相关性(r＞0.999 0),检出限为0.34 μg/kg～2.14 μg/kg,加标回收率为75.9％ ～ 112.4％,相对标准偏差(RSD)为1.1％ ～4.6％.结论 2种前处理方法中丙酮-正己烷依次提取比单独用石油醚提取效果好.该方法操作简单,快速,灵敏度和准确度高,适用于各类保健品中六六六、滴滴涕残留量的检测.

目的建立测定保健食品中叶酸含量的液相色谱法,并用于考察保健食品中叶酸的稳定性研究.方法样品中的叶酸经0.5％ 氨水热水浴20分钟提取后,经ZORBAX SB-C18(150 mm×4.6 mm,5μm)分离,流动相为磷酸盐缓冲液-甲醇(70:30,V/V),流速:1.0 mL/min;紫外检测波长为280 nm,根据保留时间定性,外标峰面积法定量.结果叶酸在4.685μg/mL～74.960μg/mL内线性关系良好(r=1),样品的加标回收率为94.8％ ～97.6％,平均回收率为96.0％,RSD为1.1％;检出限为0.18μg/mL;定量限为0.60μg/mL.样品经过3个月的加速破坏性试验后,检测其中的叶酸含量平均下降比率为2.6％.结论该方法具有操作简便快速、分离效果好、精密度和准确性高、重现性好的特点,可为叶酸类保健食品的质量控制提供方法参考.同时经稳定性试验发现样品中叶酸的含量变化不大,具有良好的稳定性.

目的 建立保健食品中石斛碱检测的气相色谱法,并用于保健食品中石斛碱的稳定性研究.方法 样品中的石斛碱经含有0.05％甲酸的甲醇回流提取后,经DB-1毛细管柱(0.25 μm×0.25 mm,30m)分离,程序升温:初始温度80℃,以10℃/min的速率升温至为250℃,保持5 min;进样口温度为250℃;FID检测器,温度为250℃;载气为N2,流速为1 ml/min;进样量为1μl;分流比为10∶1.根据保留时间定性,内标法定量.结果 石斛碱在4.395 μg/ml ～70.32 μg/ml线性关系良好(r=0.999 7),样品的加标回收率为95.5％～102.3％,平均回收率为98.1％,RSD为2.4％;检出限为0.36μg/ml;定量限为1.19μg/ml,样品经过3个月的加速破坏性试验,检测其中的石斛碱含量平均上升比率为2.2％.结论 该方法具有操作简便快速、分离效果好、精密度和准确性高、重现性好的特点,可为石斛碱类保健食品的质量控制提供方法参考.

Objective To establish a method for the determination of harmful elements pollution and trace elements in chrysomya megacephala larvae by inductively coupled plasma mass spectrometry (ICP-MS) with microwave digestion.Methods By controlling the conditions of sample microwave digestion,Pb,Cd,Hg,As,Cr,K,Na,Mg,Ca,Fe,Zn,Cu,Mn,Se from different sources of chrysomya megacephala larvaes could be determined simultaneously by ICP-MS,and the contents were detected and compared.The accuracy of the method was evaluated with standard chicken components(GBW10018) and standard liver components(GBW10051).Results The contents of harmful elements pollution in chrysomya megacephala larvae were below the limits.The differences between trace elements were significant,the contents of K,Na,Mg,Ca were the highest,Fe,Zn,Cu,Mn were the second,and Se was the lowest.Good linearity was obtained for each element(r ＞0.999 0),the detection limit of the method was within 0.003 446 μg/L-10.428 8 μg/L,with the recovery rate of 94.0％-105.9％ and RSD ＜ 5.0％.Conclusion The method was accurate,simple,rapid,sensitive and could provide reference for the detection and control of harmful elements pollution and trace elements in chrysomya megacephala larvae.

Objective To establish a method for simultaneous determination of silybin and schisandrin in health food by high performance liquid chromatography(HPLC).Methods The samples were extracted by ultrasonic extraction by methanol,target chemicals in samples were ultrasonically extracted with methanol and then were separated on Poroshell 120 EC-C18 (4.6 mm × 100 mm,2.7 μm).The mobile phase solution of methanol-water was used at a flow rate of 0.7 ml/min.The UV detection wavelengths of silybin was 287 nm and schizandrin was 250 nm.Qualification was conducted according to the retention time,and the external standard peak area was used for quantification.Results When the concentration of silybin was within 0.0 μg/ml-243.9 μg/ml,the correlation coefficient was 0.999 7,the detection limit of the method was 1.82 μg/ml,the relative standard deviation(RSD) was 0.84％ (n =6),and the recoveries of samples were within 97.4％-102.1％.When the concentration of schizandrin was within 0.0 μg/ml-43.3 μg/ml,the correlation coefficient was 0.999 6,the detection limit of the method was 0.48 μg/ml,the relative standard deviation(RSD) was 0.56％ (n =6),and the recoveries of samples were within 97.4％-102.5％.Conclusion The method is simple,fast,sensitive and accurate,and it is suitable to the determination of silybin and schisandrin in health food.

Objective To establish a method for the determination of curcumin in health food and apply the method to study the stability of curcumin in the health food.Methods Curcumin in the samples was extracted by methanol reflux,then separation was performed on an Ultimate XB-C18 column (100 mm × 4.6 mm,3 μm);the mobile phase of acetonitrile-4％ Glacial acetic acid(48:52,V/V) was used at a flow rate of 0.8 ml/min and the UV detection wavelength was set at 430 nm.Qualification was conducted according to the retention time,and the external standard peak area method was used for quantification.Results Good linearity was obtained (r =1) when the concentration of curcumin was within 4.953 5 μg/ml-79.256 0 μg/ml,the spiked recovery was within 98.0％-103.5％,the average recovery was 100.8％ and RSD was 2.0％.The lowest detection limits was 0.027 μg/ml;the limit of quantification was 0.093 μg/ml.The average decrease rate of curcumin was 1.6％ after three months of accelerated destructive test on the samples.Conclusion The method is simple,fast,reproducible with good separation effect,high precision and accuracy,which can provide reference for the quality control of curcumin in health food.Meanwhile,the content of curcumin in the sample did not changed much,which indicated its stability.

目的 统计历年我国各省市食品中食源性致病菌的污染情况.方法 引用各类文献的监测数据与保健食品的检验结果进行分析汇总.结果 在食品中,沙门菌、单核细胞增生李斯特菌、金黄色葡萄球菌、副溶血性弧菌平均检出率均较高.沙门菌在肉类中检出率最高,为12.55％.副溶血性弧菌在水产品中检出率较高,为10.91％.单核细胞增生李斯特菌在生肉中检出率较高,占6.82％.金黄色葡萄球菌在熟食中检出率为4.63％,蔬菜中检出率为3.24％.保健食品中沙门菌、志贺菌、金黄色葡萄球菌、溶血性链球菌均未检出.结论 各地区不同食品中食源性致病菌检出率存在差异.

目的 建立破壁灵芝孢子粉保健品中铅的湿法消解-石墨炉原子吸收测定方法,为保健食品质量控制提供检测依据.方法 样品经硝酸-过氧化氢消化体系与硝酸-高氯酸消化体系消解,优化原子吸收分光光度仪的原子化和灰化升温程序,比较1％磷酸二氢铵和1％磷酸二氢铵-0.06％硝酸镁基体改进剂,将最佳的基体改进剂加入到样品消化液中,调整石墨炉原子吸收分光光度仪测定的最好状态后测定.结果 测定浓度在0.0 μg/L ～ 50.0 μg/L,方法的线性关系良好,相关系数r =0.999 5,检出限为0.14 μg/L,相对标准偏差为4.6％ ～6.5％,样品的加标回收率为98％～110％.结论 该方法具有操作简单、快速简便、灵敏度和准确度高的优点,具有较高的实用性,为有效控制破壁灵芝孢子粉保健品中铅提供了依据,便于推广应用.

以正辛醇-水分配体系模拟竹叶的水煎液中Cu、Fe、Zn在人体肠胃中的分配情况,用原子吸收光谱法测定竹叶、竹叶水煎液以及水煎液中上述各元素水溶态和醇溶态的含量.初步探讨了酸度变化(人体胃肠酸度)对微量元素吸收的影响,结果表明,竹叶中微量元素的形态分布与作用靶位(胃、肠)的酸度有关.

硝酸—高氯酸(4∶1)混酸分解竹叶样品,原子吸收光谱法测定竹叶中的Cu、Fe、Zn、Ni、Pb、Cd、Cr等7种微量元素,并比较了不同地区的竹叶中微量元素的含量.结果表明,竹叶中7种微量元素含量差异显著,其中Cu、Fe和Zn的含量较高,Ni、Pb次之,Cd和Cr最低,可为竹叶的质量评价提供参考依据.

To study the inhibition of Chrysomyia Megacephala Fab larva extracts on lung cancer cell A549 and Leukemia cell HL-60. The effect of the unsaturated fatty acid, rouht fat, larva dry powder and the extracts of Chrysomyia Megacephala Fab larva on lung cancer cell A549 and Leukemia cell HL-60 were observed by cell culture in vitro using the method of MTT. When culturing HL-60 and the extracts with different concentrations, they had obvious inhibition action on cell activity with concentrations of 125,250,500 μg/ml. Data showed that the Inh% of unsaturated fatty acid was (96.2±3.6)% with a concentration of 250 μg/ ml. With the same concentration, the Inh% of unsaturated fatty acid on A549 was (97.0 ± 0.5)%. However the protein was not detected. This showed that effective component of Chrysomyia Megacephala Fab larva was fat, especially unsaturated fatty acid. LD50 of the unsaturated fatty acid was above 20 g/kg(1000-fold more than human daily dose),which afforded experiment information for low-oxic and efficient drugs of antileukemia and lung cancer.

铁缺乏和缺铁性贫血是全世界范围最常见的营养缺乏病,主要影响较大的婴儿、幼儿和育龄期妇女[1-3].增加膳食铁摄入量和提高铁的生物利用率可预防铁缺乏和缺铁性贫血.

目的:研究越橘提取物复合维生素A对改善视疲劳的作用。方法:选择视力易疲劳的受试者120名,分为试食组和安慰组,每组60人,试食组口服越橘提取物复合维生素A每日2次,每次1粒,对照组口服颜色、性状与越橘提取物复合维生素A胶囊相同的安慰剂,食用量同试食组,试验期限为30 d。然后进行下列检查:常规观察、安全性检查、眼部症状检查、观察眼部自觉症状、眼科常规检查、明视持久度测定、视力检查。结果:30 d后试食组视疲劳明显减轻,双眼明视持久度平均提高13.23%±10.34%,总有效率51.9%,对照组明视持久度平均提高1.39%±4.74%,总有效率5.8%,经统计学处理差异有显著性。结论:研究表明越橘提取物复合维生素A能有效缓解人体视疲劳。

目的:建立保健食品中壳聚糖含量的测定方法。方法:采取正交试验L9(34),优化水解工艺条件。结果:以80%H2SO4,温度95℃,时间20 m in水解效果最佳。结论:该优化条件下得到的壳聚糖水解度为92.0%,重复性试验的RSD为2.8%,回收率试验结果为96.7%~100.4%。

OBJECTIVE To study the method of heme pu rification and to detect product quality.METHOD The solvent concentration,extracting time and ratio of s olid to liquid were the three factors in the experiment,and we choose three leve ls for each factor to do the experiment by orthogonal test.The content of heme w as determined by HPLC.Finally we determined the content of heme by analysis the content of the iron.RESULTS The factor B and C had some effect on the content of he me.CONCLUSION The optimum technological conditions have been attai ned by orthogonal experiment as follows: solvent concentration is 1.5% NH 3H 2 O, ratio of solid to liquid is 1∶35and extracting time is 10min.The heme purity is more than 96%.

目的:研究复方红曲制剂对实验动物调节血脂的作用.方法:将实验大鼠分成4组,在给予高脂饲料的同时,对照组给予蒸馏水,实验组给予高、中、低剂量的复方红曲制剂,连续 28 d.结果:高、中、低剂量组(1 000、333、167 mg/kg)大鼠血清甘油三酯(TG)水平明显低于高脂对照组,低剂量组大鼠血清胆固醇(TC)水平明显低于高脂对照组.高、中、低剂量组大鼠血清高密度脂蛋白胆固醇(HDL-C)水平明显高于高脂对照组.结论:复方红曲制剂具有调节血脂的作用.

本文研究了甲鱼油中多不饱和脂肪酸的提取与纯化.采用乙酯化法提取甲鱼油中的多不饱和脂肪酸,通过正交实验确定了最佳提取条件:乙醇/甲鱼油比0.73:1,NaOH用量3%(油重),反应温度65℃,反应时间2h;采用尿素包合法纯化多不饱和脂肪酸,考察尿素用量、搅拌时间、包合次数对尿素包合率的影响,通过正交实验确定最佳纯化条件:尿素/乙醇饱和溶液:脂肪酸乙酯=15:1,搅拌时间3h,包合次数1次.实验结果表明,应用乙酯化法与尿素包合法可从甲鱼油中制得高纯度的多不饱和脂肪酸.

OBJECTIVE To extract the sphingomyelin from erythrocyte membrane and hydrolyze it to ceramide. METHOD Sphingomyelin was prepared through the process of separating erythrocyte from blood,erythrocytolysis,dehydration,dry,et al,and then hydrolyzed to ceramide by phospholipase C. RESULTS The sphingomyelin was obtained from erythrocyte membrane with this method and the ceramide was consequently obtained. CONCLUSION Sphingomyelin can be obtained from erythrocyte membrane by this method.

以粗品血红素为原料,经稀碱、稀酸处理,通过正交实验分析,确定最佳纯化条件为:提取液氨浓度为1.5%,固液比为1:35,提取时间为10 min.产品纯度大于96%,回收率大于80%,具有工艺简单、成本低廉、无污染、生产周期短等优点.