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App Notes & White Papers

Application Notes

Not Your Kids Apple Juice: An Examination of Arsenic Content in American and European Hard Ciders

Abstract:

Hard cider or alcoholic cider is an alcohol-fermented beverage produced primarily from apples. Hard ciders have a long history around the world but have only become readily available in the United States over the past two decades. Over the last several years, several studies have been conducted showing the presence of arsenic in apple juices and wine.

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How Much Lightning Is In Your Morning Jolt: A Study of the Concentration of Caffeine and Other Organic Coffee Marker Molecules in Fast Food and Home-Brewed Coffee

Abstract:

Coffee is a major world commodity with 7 million metric tons of coffee produced annually. Roasted coffee beans can contain well over a thousand different compounds. In most cases, the most important of those chemicals are the flavor compounds (i.e. chlorogenic acids, polyphenols, terpenes, etc.) and caffeine. Other compounds, such as methyl cafestol and homostachydrine, can be important in fingerprinting the authenticity and adulteration of coffee and coffee species. This study created chemical profiles of coffee around targeted groups of chemical markers in coffee to determine: caffeine content (and decaffeination by-products), coffee or species authenticity, and adulteration and safety of coffee using LC/MS. Brewed regular roast and decaffeinated coffee was purchased from multiple chain fast food restaurants, coffee purveyors and convenience stores.

 Read the Application Note(PDF)

In Pursuit of the True Value- Error and the Use of Standards in Producing Accurate Data

Abstract:

Analytical laboratories face more challenges and regulations than ever before as accreditation bodies issue increasing numbers of guidelines; and regulatory agencies increase the number of analytes that need to be reported while the levels of detection required decrease. A lot of time, effort and money is invested in deciphering the data and determining its validity and accuracy. Often terms which describe data are used incorrectly or interchangeably to try to validate a data set or methodology (i.e. error vs. uncertainty, precision vs. accuracy, etc). One of the first steps to understanding and validating data is the proper application of appropriate statistics and the understanding of the use and terminology of analytical processes.

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Lead Levels in Nutraceuticals: Spice and Cannabis Nutraceutical Hemp Products

Abstract:

The consumption of botanical products has increased over the past two decades as consumers trend to what are perceived to be natural and high quality botanical products. The cannabis industry has taken the world by storm and has flooded market with new products. Recently, concerns have arisen around the safety of this largely unregulated market. Cannabis testing laboratories emerged to fill the need for specialized testing for cannabinoid potency, pesticides, bacteria/mold, and other potential contaminants.

Toxic heavy metals are too often found in many common food and health products as well as in our environment. Products which often originate from other countries around the world can be targets for higher contamination, adulteration and counterfeiting with or by heavy metals. The primary regions of spice and tea production around the world have often been cited as having less stringent safety and quality standards in regards to consumer products. Products from these regions have been noted to contain a variety of adulterants and contaminants including wear metals and toxic elements.

Cannabis, potentially, with its mixed legal status, may be poised to become the next crop to be adulterated. Recreational cannabis and hemp are both the same species. Federally, legal hemp products are easy to obtain by the general public. Hemp products are also used as base for cannabis products and cannabinoid extracts. However, due to a ban on hemp cultivation in the US, virtually all of the hemp based in the US is imported from China, India, Eastern Europe, and Canada. Studies of other commodities exported from these countries have reported widespread heavy metal contamination (i.e. spices, teas, grains, etc.).

The scope of this study was to analyze various spice and legal hemp nutraceutical products, currently on the market, for lead contamination and compare those levels to other foodstuff and nutraceutical products examined in past SPEX CertiPrep studies. Samples were digested using microwave digestion and analyzed by ICP-OES and ICP-MS. Read the Application Note(PDF)


Analysis of Cannabis and Hemp Products for Heavy Metals

Abstract:

The cannabis industry has taken the world by storm and has flooded the market with new products. Recently, concerns have arisen around the safety of this largely unregulated market. Cannabis testing laboratories emerged to fill the need for specialized testing for cannabinoid potency, pesticides, bacteria/mold and other potential contaminants. Sadly, a significant group of contaminants has been largely ignored: toxic metals.

Recreational cannabis and hemp are both the same species. Federally legal hemp products are easy to obtain by the general public. Hemp products are also used as base for cannabis products & cannabinoid extracts. However, due to a ban on hemp cultivation in the US, virtually all of the hemp used in the US is imported from China, India, Eastern Europe, and Canada. Studies of other commodities exported from these countries have reported widespread heavy metal contamination (i.e. spices, teas, grains, etc.).

Cannabis plants are potential bioaccumulators of heavy metals. In the production of these products, a large amount of plant material is processed to extract concentrates and oils, thereby increasing the risk of heavy metal contamination. The scope of this study was to analyze various legal hemp products, currently on the market, for heavy metal contamination and use hemp as a model for methods development for restricted products. Samples were digested using microwave digestion and analyzed by ICP-OES and ICP-MS. Read the Application Note(PDF)


The Reality of Cannabis Testing: Thinking Outside the Bud

Abstract:

It seems that every week new information is being released about the regulations of cannabis in the United States. Recently, with the legislation opening up a new agricultural and testing industry around cannabis, labs are now on the forefront of testing and legislation. The science and regulatory communities are now defining the roles and targets for testing in this new industry, as well as redefining global testing strategies for testing harmonization all over the world. The legalization of cannabis in certain states has started a gold rush of growing facilities and testing labs all trying to shape law and regulation out of what was previously an unregulated, illegal product. Read the Application Note(PDF)


Elemental Content of Black Pepper to Determine Adulteration and Heavy Metal Contamination

Abstract:

The consumption of botanical products has increased over the past two decades as consumers trend to what are perceived to be natural and high quality botanical products. The primary regions of spice and tea production around the world have often been cited as having less stringent safety and quality standards in regards to consumer products. Products from these regions have been noted to contain a variety of adulterants and contaminants including wear metals and toxic elements. The most traded spice in the world is black pepper and accounts for 20% of the world spice market. It is also one of the most commonly adulterated spices on the marketplace with up to 70% of commercial black pepper samples showing some form of adulteration or counterfeiting.

Black pepper samples were purchased at dollar stores, farmers markets, chain stores, and online vitamin outlets. Products selected included both whole black peppercorns and ground black pepper sold as both retail and organic products. Physical and chemical screening methods were used to detect gross adulteration and counterfeiting. ICP was used to determine the macroelement components (Si, Na, Mg, Fe, and K) that indicated possible adulteration or contamination. High levels of bulking agents, including silica and sodium, were often found in low cost spices indicating potential adulteration. ICP-MS was used to determine the presence and level of heavy metal contamination and adulteration. The black pepper samples had many examples of high heavy metals content at the ppm level, including high lead and chromium levels, which could be indicative of adulteration by lead chromate or lead oxides.

The United States Department of Agriculture (USDA) maintains an extensive database of chemical and physical data for food products. These databases show the normal distribution of values of nutritional components for spices. The black pepper samples were compared to the USDA values to determine if their composition was within the normal distribution for a black pepper spice. Many samples were identified with a high probability of adulteration or counterfeiting since they did not fit the spice profile. Read the Application Note(PDF)


Heavy Metal Contamination of Red Pepper Spices and Hot Sauce

Abstract:

The consumption of botanical products has increased over the past two decades as consumers trend to what are perceived to be natural and high quality botanical products. The primary regions of spice and tea production around the world have often been cited as having less stringent safety and quality standards in regards to consumer products. Products from these regions have been noted to contain a variety of adulterants and contaminants including wear metals and toxic elements.

The spice samples used were purchased at dollar stores, farmer’s markets, chain stores, and online vitamin outlets. Products included organic products. Cryogenic grinding and microwave digestion were employed in sample processing. ICP-MS was used to determine the presence and level of heavy metal contamination and adulteration. Read the Application Note(PDF)


Examination of Pesticides in Wine, Beer and Their Constituent Products Using High-Throughput Techniques to Maximize Extraction & Efficiency

Abstract:

There are hundreds of commercial pesticides in use in industrial and private agriculture. Concern over the health effects of residual pesticides on fruits and vegetables has led to increased testing of these products to determine the levels of pesticides on produce when it goes to market.

In this study, commercial red wine and beer samples were examined for their pesticide concentrations. In addition to the examination of the finished alcoholic beverage, the constituent agriculture products of wine and beer production (grains, malts hops and wine grapes) were also examined to determine the levels of pesticides found in those products. The sample preparation and extraction process efficiency and recovery were examined by processing samples using manual versus high-throughput techniques. The QuEChERS method was used to process a greater number of samples in a shorter period of time than other extraction methods. Read the Application Note(PDF)


Sample Preparation, Extraction and Analysis of Imported Children's Toys for Bisphenol A and Phthalates

Abstract:

The US has started to limit levels of some phthalates for use in children’s’ products including DEHP, DBP, BBP, DINP, DIDP & DIOP. The Consumer Product Safety Commission (CPSC) has published testing methods for these regulated phthalates. The regulation of bisphenol A (BPA) remains under debate. This study examined the levels of phthalates and BPA in 26 children’s toys purchased from local discount or ‘dollar’-type stores. The toys were all reported as being made in China.

Microwave extraction methods were created and optimized against SPEX CertiPrep certified solid reference materials to compare levels of phthalates and BPA found in the toys. Samples were examined using GC/MS. High levels of phthalates and BPA were detected in the majority of the PVC toys. In many samples the concentration of phthalates far exceeded the limits set by the CPSC. Read the Application Note(PDF)


Analysis of Laboratory Water for BPA and Phthalates

Abstract:

Phthalate and bisphenol A (BPA) levels were studied in municipal water straight from the tap and processed through drinking water treatment systems as well as various samples of laboratory water from commercial sources and from deionized (DI) filtration systems. Samples were extracted and tested by GC/MS. The water samples taken directly from municipal tap water had relatively small concentrations of phthalates and BPA but when decanted through consumer Point of-Use (POU) drinking water filtration systems, the level of phthalates and BPA varied greatly depending on the type of system and the amount of water flushed from the system prior to the sample being taken. Laboratory water sources appeared to have the greatest variability on phthalate concentration with LC/MS grade water having the lowest phthalate and BPA concentrations of all the laboratory water. Read the full Application Note(PDF)


Analysis of Gourmet Salts for the Presence of Heavy Metals

Abstract:

Salt has been a common commodity and household staple for thousands of years. Over the past decade salt has transformed from common product into a gourmet item with various origins, processing methods, representing all the colors and flavors of the gourmet spice market. Gourmet salt sales exceed $250 million dollars a year. Some exotic varieties are luxury products retailing for more than $20 an ounce compared to regular table salt at $0.02 an ounce.

This study examined a variety of gourmet salts for the elemental composition and for the presence of heavy metals. The salt samples represented many different colors, production methods, textures and price points. Read the full Application Note(PDF)


Analysis of Lipstick for Toxic Elements Using ICP-MS

Abstract:

Evidence of the use of cosmetics, including lipstick, has been found in civilizations as early as ancient Mesopotamia. Many of the cosmetics used throughout history have contained potentially toxic elements and other contaminations. Ancient Egyptians used cosmetics containing large amounts of lead and mercury. Modern cosmetics are perceived to be free of dangerous toxins due the widespread regulation of many consumer products. The FDA, which oversees the regulation of cosmetic products, does not have regulations governing the level of toxic or dangerous contaminants in finished products such as lipsticks.The FDA regulates limits on compound concentrations of additives and colorants but no overall regulation is in place for the finished product’s level of potential contamination.

Studies prior to 2012, have found levels of lead up to 3 ppm in lipstick. The purpose of this study was to re-examine the potential for lead contamination in lipstick and determine if any other potentially toxic metals were present in these lipsticks. Forty-eight lip products including lipsticks, lip glosses, moisturizing sticks, and lip stains were tested for the presence of toxic elements by ICP-MS. Read the full Application Note(PDF)


Analysis of Elemental Content in Commercial Chocolate Bars

Abstract:

Chocolate has been harvested for human consumption for thousands of years. The Mayans used cocoa beans as currency. Present day consumption of chocolate is measured on a global scale. In the US, Americans consume over 11 pounds of chocolate per person per year.

Cocoa plants are native to tropical climates with high levels of humidity and rainfall. This climate increases the need for pesticide application to protect the cocoa bean crops. Heavy metals from pesticide and fertilizer applications can accumulate in the soil and add to the possible accumulation of those metals in the cocoa beans.

This study examined the elemental composition of several types of chocolate products from chocolate liquor to milk and dark chocolate bars. Read the full Application Note(PDF)


The Effect of Heat Exposure on BPA and Phthalate Content in Commercial Bottled Water

Abstract:

The goal of the present study was to examine the phthalate and bisphenol A (BPA) levels of several popular commercial bottled waters in comparison with municipal tap water. In addition, the study attempted to discover whether the phthalate and BPA levels increased after being heated one week at temperatures equivalent to those reached inside an automobile during the summer (60° C). Samples were extracted and tested for phthalate and BPA levels by GC/MS. The concentration of phthalates and BPA found in all the commercially bottled water samples and the municipal water source were either non-existent or well below established guidelines. In addition, the exposure of bottled water to heat did not significantly increase the concentration of phthalates. BPA was not detected in any of the bottled water or municipal water source. Read the full Application Note(PDF)


 

Trace Elements in Fish Oil and Fish Oil Supplements

Abstract:

For years, the American Heart Association has recommended eating an average of two to three fishmeals each week to help reduce cholesterol, high blood pressure, and hardening of arteries. Research shows that consuming fish increases high quality protein with fewer calories, and it is rich in omega-3 fatty acids. Omega-3 fatty acid helps to reduce the risk of coronary artery disease, helps in the treatment of bipolar disorder/depression, and helps reduce inflammation in autoimmune diseases (1,4). Fish are also low in sodium and a good source of potassium. Some examples of fatty, coldwater fish that are high in omega-3 fatty acids include salmon, mackerel, and herring.

Unfortunately, due to industrial pollution, many fish have high levels of contaminants including mercury, methyl mercury, and PCBs (polychlorinated biphenyls), which are absorbed by surrounding waters and from foods they eat. Currently, the EPA limit for mercury in fish is 1 ppm. About 22% of all PCBs are in estuarine and coastal sediments, which accounts for 95% of the fish production (2). The EPA estimates up to 15% of mercury emissions from these utilities fall within 30 miles of a plant, and up to 50% falls within six hundred miles. The mercury bio-accumulates through the food chain and reaches the predator species. For example, a Nevada reservoir fish tissue sample shows an average of 0.47 ppm mercury; the EPA guidelines recommend limiting consumption of such fish to one 8-ounce meal per month for adults (3).

For humans, mercury and methyl mercury are toxic and can damage the brain and the nervous system.Mercury poisoning symptoms include numbness in hands and feet, general muscle weakness, and vision, hearing, and speech damage. In extreme cases, insanity, paralysis, coma, and death follow. The U.S. Food and Drug Administration and the EPA advised pregnant women and those who might become pregnant to avoid certain fish known to be high in mercury. This study will investigate trace element concentrations including heavy metal concentrations in different types of fish and fish oil supplements available from local markets in New Jersey. Read the full Application Note (PDF)


Examination of Commercial Botanical Products for Presence of Heavy Metals by ICP-MS

Abstract:

The consumption of botanical products has increased over the past two decades as consumers trend to what are perceived to be natural and high quality botanical products. The primary regions of spice and tea production around the world have often been cited as having less stringent safety and quality standards in regards to consumer products. Products from these regions have been noted to contain a variety of adulterants and contaminants including wear metals and toxic elements.

Common botanicals (black and red pepper, cinnamon, mustard, cumin, and turmeric) sold as spices, teas, condiments, and supplements were purchased at dollar stores, farmers markets, chain stores, and online vitamin outlets. Products selected covered the range of preparations includin gground species, blends, supplement teas and sauces (retail and organic) products. Physical and chemical screening methods were used to detect gross adulteration and counterfeiting. ICP was used to determine macroelement components (Si, Na, Mg, Fe, and K) that indicated possible adulteration or contamination. High levels of bulking agents, including silica and sodium, were often found in low cost spice and botanical samples indicating potential adulteration. ICP-MS was used to determine the presence and level of heavy metal contamination and adulteration. Most of the spice groups studied had many examples of high heavy metals content at the ppm level including very high lead levels which could be indicative of adulteration by lead chromate or lead oxides. Read the full Application Note (PDF)


Analysis of Organic Marker Compounds and Hazardous Organic Compounds by GC/MS to Identify Contamination, Counterfeiting and Adulteration of Spices

Abstract:

Food adulteration and counterfeiting continues to grow as a worldwide issue of food safety and economic concern. Spices are one of the most commonly adulterated and counterfeited agricultural products in the US. Our previous study determined extensive elemental and heavy metals contamination and adulteration in spices. Many of our spice products were identified as possibly being highly adulterated or contaminated by metals. In our follow-up organic study, we focused on the organic markers and toxic organic compounds in our common spices and botanicals (black pepper and cinnamon) in various forms (i.e. spices, teas, condiments, and supplements) to determine if tehse products appeared to be adulterated from an organic compound standpoint as well as an elemental standpoint.

Cryogenic grinding and microwave extraction were employed in sample processing. Samples were extracted for the primary and secondary marker compounds native to each spice group and for any potentially toxic organic compounds (dyes, preservatives, pesticides, and industrial residual chemicals). The concentration and identity of compounds were compared across the groupings to cited concentration references for each marker or compound. Low concentrations of critical markers were found in low cost spice and botanical samples indiciating potential adulteration. Samples that were previously suspect by ICP-MS examination were confirmed to be adulterated or economically compromised by reduced or absent concentration of these critical primary and secondary marker compounds. High levels of potentially toxic chemicals were also found in some of the previously suspect spice and spice product samples.  Read the full Application Note (PDF)


 

White Papers

A Statistical Approach to Reporting Uncertainty on Certified Values of Chemical Reference Materials for Trace Materials

Abstract:

This article discusses an approach by a manufacturer of Calibration Standards and Certified Reference Materials to standardize the reporting of uncertainty associated with certified values quoted on a Certified Reference Material certificate of analysis. The method, based on well-established principles, relies on the authors’ belief that to report accurate and reliable certified values, it is essential to determine the value in the final solution by two independent analytical methods - usually one instrumental technique such as inductively coupled plasma-optical emission spectrometry (ICP-OES) or inductively coupled plasma-mass spectrometry (ICP-MS), and one traditional wet chemical technique - both traceable to a standard reference material. Read the full White Paper(PDF)


The Analysis of Laboratory and Consumer Water Sources for the Presence of BPA and Phthalates

Abstract:

Bottle water is a multibillion dollar a year business with projected growth to over $168 billion dollars in sales worldwide by 2012. It has gone from a designer fad in the 1980's and 1990's to a mainstay of the world consumer experience. In 2007, the average American drank over 29 gallons of bottled water. Overall, the U.S. consumed over 8.8 billion gallons of bottled water. Bottled water has become the second largest consumed beverage in the country, behind carbonated beverages. The main reasons that Americans give for drinking bottled water were first they were substituting bottled water for other beverages and second, they were concerned about the safety of their tap water. In many countries, especially developing nations, consumers buy bottled water as a safe alternative to their existing water sources. The regulation and monitoring of bottled waters in developing countries can be non-existent or less stringent than regulations in more developed nations.

The goal of this study was to examine currently debated topics regarding BPA and phthalate exposure in consumer water sources such as: 1. Are BPA and/or phthalates present in consumer bottled water? 2. Does the exposure of commercial bottled water to summer temperatures increase the leaching of BPA or phthalates into that water? 3. Are the levels of phthalates and BPA in municipal or filtered water samples significantly different than the levels found in bottled water? Read the full White Paper(PDF)


ICP, ICP/ICP-MS, and ICP-MS Grade Certified Reference Materials: Is There Really a Difference?

Abstract:

A blind laboratory study was conducted to compare standards obtained from various manufacturers of certified reference materials. There are two goals for this study: First to objectively determine if a difference exists between an ICP grade standard and an ICP-MS grade standard and second to focus on the equivalency of the ICP-MS grade standard to the ICP/ICP-MS grade of standard.

The single element standard selected for study was 1000 ppm Iron, due to its popularity and known interferences. ICP-MS standards were obtained whenever possible directly from the manufacturer; if this was not possible alternate sources were used. A total of 13 single element Fe standards were analyzed. Two of these were ICP-MS grade standards, five were ICP grade standards, and six were stated for use on either an ICP or ICP-MS instrument.

The multi-element solutions were selected to be similar to the SPEX CertiPrep CLMS-2 Claritas PPT ICP-MS standard. See Table 1 for the contents of CLMS-2. This standard was selected since it contains many elements commonly analyzed by ICP-MS. All of the multi-element solutions studied were ICP-MS grade. Read the full White Paper(PDF)


Guide for Determining ICP/ICPMS Method Detection Limits and Instrument Performance

Abstract:

As the term itself implies, one cannot make a measurement below the detection limit. But not everyone has a complete understanding of what the true detection limit is or how it is determined. So what is the method detection limit (MDL)? Read the full White Paper(PDF)

 
 

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