加速溶剂提取-高效液相色谱法测定蜜饯中6种食品添加剂的含量

目的:建立了加速溶剂萃取技术提取-高效液相色谱分析蜜饯中苯甲酸、山梨酸、胭脂红、苋菜红、安赛蜜、糖精钠的方法。方法:优化了压力、温度、静态时间、循环次数等参数。加速溶剂萃取提取蜜饯中添加剂的条件是:萃取温度80℃,压力10.3 MPa,静态提取6 min。结果:6种添加剂在0.02 mg/L～50 mg/L范围均具有良好的线性,相关系数均大于0.999,检出限分别为4.7μg/L～7.8μg/L,回收率分别为89%～99%,RSD均小于5.0%。结论:实验结果表明,该方法灵敏度高,重现性好,准确度高,可满足食品中添加剂分析。     

高效液相色谱荧光检测法同时测定婴幼儿食用鱼粉中环丙沙星和恩诺沙星残留量

目的:建立用高效液相色谱荧光检测器同时测定婴幼儿食用鱼粉中环丙沙星和恩诺沙星残留的方法。方法:试样经水复原后,由5%乙酸乙腈提取,正己烷脱脂,以0.05 mol/L磷酸三乙胺缓冲液-乙腈(体积比为85∶15)为流动相洗脱,荧光检测器定性定量。结果:该方法对测定的两种药物的检出限均为5μg/kg,定量限均为10μg/kg。两种药物在5μg/L~80μg/L范围内线性关系良好,相关系数均大于0.99。在添加水平分别为10μg/kg、20μg/kg和80μg/kg时,两种药物的加标回收率为80.3%~92.6%,相对标准偏差(RSD)为1.2%~3.8%。结论:方法操作简单、重现性好、灵敏度高、分析时间短,适用于鱼粉中环丙沙星和恩诺沙星残留的确证检测。     

自动顶空毛细管柱气相色谱法测定生活饮用水中的5种卤代烷烃

目的建立同时测定生活饮用水中5种卤代烷烃的自动顶空毛细管柱气相色谱法。方法准确吸取2 ml水样于顶空瓶中,顶空装置自动进样,毛细管柱分离,GC-ECD进行检测。结果水样中5种卤代烷烃均在14 min内完成检测,线性范围分别为:三氯甲烷:0μg/L~4.24μg/L;四氯化碳:0μg/L~1.2μg/L;一氯二溴甲烷:0μg/L~5.24μg/L;二氯一溴甲烷:0μg/L~3.72μg/L;三溴甲烷:0μg/L~12.36μg/L;相关系数r0.999,检出限为0.065μg/L~0.51μg/L;两组混标样的添加回收率均为94.4%~105.6%,相对标准偏差(RSD)均5%。气相色谱柱温条件:初始柱温为60℃,保持5 min,之后以10℃/min升温至85℃,保持7 min。顶空进样装置保温时间为15 min。结论该方法具有简便快速、检出限较低、线性关系较好、回收率高等特点,适用于生活饮用水中三氯甲烷、四氯化碳、一氯二溴甲烷、二氯一溴甲烷和三溴甲烷的检测分析。     

共振光散射法测定磺胺类药物

目的:建立测定痕量磺胺类药物的新方法.方法:基于磺胺类药物-亚硝酸根-8-羟基喹啉的重氮化-偶联反应.偶联反应产物使得468 am处共振散射光强度明显增加,从而建立了测定磺胺类药物的新方法.结果:磺胺、磺胺噻唑、磺胺甲恶唑和磺胺甲嘧啶的线性范围分别是:10～1500μg/L、50～1500 tLg/L、10～1500μg/L、10～1500μg/L;检出限分别为:8.3、12、7.9.9.1μg/L;回收率为99.9%～101.1%.结论:方法的灵敏度高,线性范围宽,用于复方新诺明中磺胺甲恶唑含量的测定,结果满意.     

基于QuEChERS测定鸡肉中22种磺胺类药物残留

目的 建立基于QuEChERS结合液相色谱-串联质谱快速测定鸡肉中22种磺胺类药物残留的方法。方法 通过对流动相的种类、提取溶剂的种类、盐析剂、吸附剂的种类和用量、定容液的种类进行讨论，在加标量为10μg/kg的条件下，改变各优化条件，以回收率为指标得出最优的前处理条件。并分析该方法的基质效应、线性关系、检出限、定量限、加标回收率和相对标准偏差(RSD),以评价方法的可行性。最后将该方法用于实际样品的检测。方法以甲醇和0.1%甲酸水溶液为流动相，样品经1%甲酸乙腈提取，2 g氯化钠(NaCl)为盐析剂，20 mg C₁₈,10 mg PSA为净化剂，经LC-MS/MS检测，用基质匹配曲线内标法定量。结果 22种磺胺类药物在0.1μg/L～20μg/L内的线性相关系数均大于0.998 8,方法检出限与定量限分别为0.11μg/kg～1.66μg/kg和0.35μg/kg～2.23μg/kg。在2μg/kg、10μg/kg、50μg/kg 3个加标水平上，平均回收率为75.6%～124.0%,RSD为1.1%～15.7%。结论 本方法快速简便、准确可靠，可用于鸡肉中的...     

湿法消解砷铈催化分光光度法测定奶粉中碘含量的方法研究

目的建立简便快速消解奶粉样品,实现其总碘含量测定的方法。方法用高氯酸、氯酸钾混合湿法消解样品溶液2小时,用砷铈催化分光光度法测定其碘含量。由吸光度值与碘浓度的对应关系,计算出样品中碘的含量。结果检测范围0~100μg/L,标准曲线相关系数为-0.999 6~-0.999 9;精密度:测定奶溶液样品中碘含量为20.11μg/L、60.45μg/L和86.55μg/L时,变异系数(CV)分别为2.54%、1.85%和1.58%;准确度:对低、中、高3种不同浓度碘含量的奶粉溶液加标回收率分别为98.90%、101.02%和99.66%(n=6),平均回收率为99.86%。结论本方法适合应用于奶粉中总碘的含量测定。     

加速溶剂萃取/凝胶渗透色谱/气相色谱-质谱法测定水果中的农药残留

目的建立简单、准确测定水果中7种有机磷农药残留的分析方法。方法取水果样品以丙酮为提取剂经加速溶剂萃取装置(ASE)萃取,提取液无水硫酸钠除水后,在线定量浓缩(EVA),再经全自动凝胶渗透色谱仪(GPC)净化,净化液在线浓缩定容后采用气相色谱-质谱法同时进行分离和定性,外标法定量检测。结果该实验条件下,7种有机磷化合物的线性关系良好,相关系数均0.999;样品加标的平均回收率为80%~118%,相对标准偏差均5.0%,该方法的检测限为0.012μg/L~0.084μg/L。结论该方法的提取效率高,稳定性好,准确灵敏,大量实际样品的检测结果表明,此方法适于水果中农药残留检测实际工作的需要。     

氧化型染发剂中12种风险组分的加速溶剂萃取-气相色谱质谱-内标测定法

目的开发氧化型染发剂中12种风险组分的加速溶剂萃取-气相色谱质谱(GC-MS)-内标测定法,研究样品加速溶剂萃取最佳操作条件。方法样品加入石英砂、亚硫酸钠、硅酸镁混合后,使用乙酸乙酯溶剂,在压力10.0 MPa,温度100℃下,静态萃取5 min,循环1次。萃取结束后氮吹浓缩,定容过滤后供GC-MS测定,内标法定量。结果样品在1.0～100.0μg/mL浓度范围内线性关系良好,相关系数r=0.992 0～0.999 6;最低检出浓度0.08～0.40 mg/kg;平均回收率为81.0%～101.5%;相对标准偏差(RSD)在1.95%～6.27%之间。结论该方法分析简单、快速、准确,可用于氧化型染发剂风险组分检测。     

加速溶剂萃取高效液相色谱-电感耦合等离子体质谱测定海产品中砷形态方法研究

目的建立加速溶剂萃取(PLE)与高效液相色谱-电感耦合等离子体质谱(HPLC-ICP MS)联用测定海产品中砷形态的方法,为食品安全风险监测提供参考方法。方法以50%甲醇-水为溶剂,采用快速溶剂萃取仪提取各形态的砷;利用阴离子交换柱分离,以O2为动态反应气消除质谱干扰,实现了As B、As(Ⅲ)、DMA、MMA、As(Ⅴ)5种形态砷的分离测定。结果 5种砷浓度在2.5μg/L~25μg/L时线性相关系数均≥0.999 0,检出限为0.1μg/L~0.2μg/L,相对标准偏差3.5%。实际样品加标回收率在80.1%~104.0%。结论方法具有快捷、准确、灵敏等优点,可分别用于无机砷、有机砷的测定,并可最大程度保留食品中砷的原始形态,便于进行形态分布研究。     

HPLC法同时测定牛奶中7种磺胺类药物和4种氟喹诺酮类兽药

目的:建立了一种同时测定牛奶中两类共11种兽药(7种磺胺类药物和4种氟喹诺酮类药物)残留量的高效液相色谱分析。方法:样品经水-乙腈(V∶V=1∶1)提取,过C-18固相萃取柱净化,残余物用流动相定容至1 ml,以乙腈和磷酸二氢钾溶液作为流动相,采用梯度洗脱程序进行液相色谱分离,用紫外检测器进行定性和定量分析。结果:磺胺类药物和氟喹诺酮类药物在0μg/ml~50μg/ml范围均具有良好的线性,相关系数均大于0.999,检出限(S/N)分别为1.3和0.8μg/L,添加水平为30,4μg时,11种兽药的平均回收率分别为88.56%~91.65%和87.25%~91.57%,RSD均小于10%。结论:实验结果表明,该方法灵敏度高,重现性好,准确度高,可满足动物源性食品中磺胺和氟喹诺酮类药物的残留分析。     

Factors associated with changes in satisfaction with care

OBJECTIVE: Satisfaction with care is an important outcome for evaluating the effectiveness of medical care. Many factors can influence satisfaction, including disease state, healthcare utilization, and health-status changes. However, few studies have investigated the association between these factors and changes in satisfaction. DESIGN: This study examined the influence of personal characteristics, type of health plan, disease states, and healthcare utilization on changes in satisfaction with care in a prospective cohort over a 12-month period through two surveys, baseline and follow-up. PARTICIPANTS: Enrollees in one of three different commercial health plans: point-of-service product, an unrestricted fee-for-service product, and a preferred-provider organization product. MEASUREMENTS AND MAIN RESULTS: Two multivariate logistic regression models were constructed. The first model evaluated factors that predicted increased satisfaction with care between the two surveys. Compared with respondents who reported no change in health status, both those with improved health status (odds ratio [OR], 1.29, 95% confidence interval [CI95], 1.03-1.61) and those with declines in health (OR, 1.29, CI95, 1.03-1.61) were significantly more likely to report an increase in satisfaction with care. Those with a history of hospitalization were also more likely to report an increase in satisfaction with care (OR, 1.27, CI95, 1.01-1.59). The second multivariate logit model evaluated factors that predicted decreases in satisfaction with care from the baseline survey. Those with reported declines in health status were more likely to report decreases in satisfaction with medical care (OR, 1.43, CI95, 1.13-1.79). Neither age, gender, race, type of health plan, disease state, nor doctor's office visits were related to observed changes in satisfaction with medical care. CONCLUSION: Changes in satisfaction with care appear to be related to changes in health status. However, the relation between these two attributes is not intuitively apparent.     

Soy isoflavones in conjunction with radiation therapy in patients with prostate cancer

Soy isoflavones sensitize prostate cancer cells to radiation therapy by inhibiting cell survival pathways activated by radiation. At the same time, soy isoflavones have significant antioxidant and anti-inflammatory activity, which may help prevent the side effects of radiation. Therefore, we hypothesized that soy isoflavones could be useful when given in conjunction with curative radiation therapy in patients with localized prostate cancer. In addition to enhancing the efficacy of radiation therapy, soy isoflavones could prevent the adverse effects of radiation. We conducted a pilot study to investigate the effects of soy isoflavone supplementation on acute and subacute toxicity (≤6 mo) of external beam radiation therapy in patients with localized prostate cancer. Forty-two patients with prostate cancer were randomly assigned to receive 200 mg soy isoflavone (Group 1) or placebo (Group 2) daily for 6 mo beginning with the first day of radiation therapy, which was administered in 1.8 to 2.5 Gy fractions for a total of 73.8 to 77.5 Gy. Adverse effects of radiation therapy on bladder, bowel, and sexual function were assessed by a self-administered quality of life questionnaire at 3 and 6 mo. Only 26 and 27 patients returned completed questionnaires at 3 and 6 mo, respectively. At each time point, urinary, bowel, and sexual adverse symptoms induced by radiation therapy were decreased in the soy isoflavone group compared to placebo group. At 3 mo, soy-treated patients had less urinary incontinence, less urgency, and better erectile function as compared to the placebo group. At 6 mo, the symptoms in soy-treated patients were further improved as compared to the placebo group. These patients had less dripping/leakage of urine (7.7% in Group 1 vs. 28.4% in Group 2), less rectal cramping/diarrhea (7.7% vs. 21.4%), and less pain with bowel movements (0% vs. 14.8%) than placebo-treated patients. There was also a higher overall ability to have erections (77% vs. 57.1%). The results suggest that soy isoflavones taken in conjunction with radiation therapy could reduce the urinary, intestinal, and sexual adverse effects in patients with prostate cancer.     

Falling in love with romantic ideals: women in relationships with child molesters

Drawing on data from a larger research study, this paper explores intersecting and competing social relations that influenced the romantic desires of women who became intimately involved with men who molested children. Through a feminist poststructuralist lens, women’s narratives were analysed with the use of feminist interpretations of Foucauldian discourse theory. Analysis informed of a discursive power over participants that made the attainment of romantic desires an imperative for ensuring social respect, worth and credibility as women. When all was not ideal, these same romantic desires compelled women to fix and hold onto their relationships – even when with men that attract damning societal responses towards them. Even upon acknowledgement of their partners’ sexual transgressions, the fear of relationship breakdown meant that romantic desires again featured as imperatives for the women. The imagined pleasure of achieving romantic desires is discursive; so powerful that it outweighed women’s fears and dangers of precarious intimate life with men who commit abhorrent acts.     

Factors Associated with Sarcopenia in Patients with Colorectal Cancer

Introduction; Sarcopenia are frequently observed in cancer patients and was associated with poor prognosis. Objectives; to determine the association of nutritional status, body composition, and clinic parameters with sarcopenia in patients with colorectal cancer (CRC). Methods; We conducted a cross-sectional study of 197 patients with CRC. The sarcopenia elements, including lumbar skeletal muscle index (SMI), handgrip strength, and gait speed were measured. The SMI was assessed by computed tomography at third lumbar vertebra. Phase angle (PA), serum albumin (SAlb), muscle attenuation (MA), and the scored patient-generated subjective global assessment (PG-SGA) were also evaluated. Univariate and multivariate analysis of factors associated with sarcopenia were performed. Results; Sarcopenia was present in 29 of 195 patients (15%) and was significantly correlated with advance age, lower body mass index (BMI), SAlb, PA, MA, higher PG-SGA score, and malnutrition (PG-SGA B). In univariate analysis, age, BMI, SAlb, PA, MA, PG-SGA score, and malnutrition (PG-SGA B) were associated with sarcopenia. Multivariable analysis revealed that BMI, SAlb, PA, MA, and PG-SGA score were independent predictors of sarcopenia. Conclusion; BMI, SAlb, PA, MA, and PG-SGA score were independent predictors of sarcopenia in patients with CRC.